Search results for: FTIR spectroscopy

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

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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: Gul Afreen, Sreedevi Upadhyayula, Mahendra K. Sunkara

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One-dimensional (1D) nanostructures like nanowires, nanotubes, and nanorods find variety of practical application owing to their unique physico-chemical properties. In this work, TiO₂ nanowires were synthesized by direct oxidation of titanium particles in a unique microwave plasma jet reactor. The prepared TiO₂ nanowires manifested the flexible features, and were characterized by using X-ray diffraction, Brunauer-Emmett-Teller (BET) surface area analyzer, UV-Visible and FTIR spectrophotometers, Scanning electron microscope, and Transmission electron microscope. Further, the photodegradation efficiency of these nanowires were tested against toxic organic dye like methylene blue (MB) and the results were compared with the commercial TiO₂. It was found that TiO₂ nanowires exhibited superior photocatalytic performance (89%) as compared to commercial TiO₂ (75%) after 60 min of reaction. This is attributed to the lower recombination rate and increased interfacial charge transfer in TiO₂ nanowire. Pseudo-first order kinetic modelling performed with the experimental results revealed that the rate constant of photodegradation in case of TiO₂ nanowire was 1.3 times higher than that of commercial TiO₂. Superoxide radical (O₂˙⁻) was found to be the major contributor in the photodegradation mechanism. Based on the trapping experiments, a plausible mechanism of the photocatalytic reaction is discussed.

Keywords: Heterogeneous catalysis, photodegradation, reactive oxygen species, TiO2 nanowires.

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Authors: M. B. Shuai, S. Xiao, Q. S. Li, M. F. Chu, X. F. Yang

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Ambient hydrolysis products in moist air and hydrolysis kinetics in argon with humidity of RH1.5% for polycrystalline LiH powders and sintered bulks were investigated by X-ray diffraction, Raman spectroscopy and gravimetry. The results showed that the hydrolysis products made up a layered structure of LiOH•H2O/LiOH/Li2O from surface of the sample to inside. In low humid argon atmosphere, the primary hydrolysis product was Li2O rather than LiOH. The hydrolysis kinetic curves of LiH bulks present a paralinear shape, which could be explained by the “Layer Diffusion Control" model. While a three-stage hydrolysis kinetic profile was observed for LiH powders under the same experimental conditions. The first two sections were similar to that of the bulk samples, and the third section also presents a linear reaction kinetics but with a smaller reaction rate compared to the second section because of a larger exothermic effect for the hydrolysis reaction of LiH powder.

Keywords: Hydrolysis, lithium compound, polycrystallinelithium hydride

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Authors: Daniella R. Mulinari, Araujo J. F. Marina, Gabriella S. Lopes

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Natural fibers are used in polymer composites to improve mechanical properties to replace inorganic reinforcing agents produced by non-renewable resources. The present study investigates the tensile and flexural behaviors of palm fibers-high density polyethylene (HDPE) composite as a function of volume fraction. The surface of the fibers was treated by mercerization treatments to improve the wetting behavior of the apolar HDPE. The treatment characterization was obtained by scanning electron microscopy, X-Ray diffraction and infrared spectroscopy. Results evidences that a good adhesion interfacial between fibers-matrix caused an increase strength and modulus flexural as well as tensile strength in the modified fibers/HDPE composites when compared to the pure HDPE and untreated fibers reinforced composites.

Keywords: Mechanical properties, palm fibers, polymer composites, surface treatment.

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Authors: S. Sumathi, V. Sethuprakhash, W. J. Basirun

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This study was focused on polymer electrolytes containing methanesulfonic acid (MSA) and p-toluene sulfonic acid (pTSA) mixed with polyacrylamide (PAAm) respectively. Impedance Spectroscopy technique has been employed to compare the ionic conductivity of these polymer electrolytes. The ionic conductivity of the PAAm hydrogel electrolytes increase upon adding the sulfonic acids. Ionic conductivity of PAAm-pTSA is higher than PAAm-MSA. The electrochemical performance evaluations were done with the tin-air cells discharge at zero current for 30minutes and at constant current density of 2.5, 5, 7.5, 10, 12.5 and 15mA/cm². The tin-air cell of PAAm-MSA produce higher specific discharge capacity compared to PAAm-pTSA. Open-circuit voltage measurement revealed a higher voltage for tin-air cell of PAAm-MSA which is 1.27V.

Keywords: Methane sulfonic acid, polyacrylamide, polymer gel electrolytes, p-toluene sulfonic acid.

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Authors: Alaaddin Cerit, Suheyla Kocaman, Ulku Soydal

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During the past two decades, photoinitiated polymerization has been attracting a great interest in terms of scientific and industrial activity. The wide recognition of UV treatment in the polymer industry results not only from its many practical applications but also from its advantage for low-cost processes. Unlike most thermal curing systems, radiation-curable systems can polymerize at room temperature without additional heat, and the curing is completed in a very short time. The advantage of cationic UV technology is that post-cure can continue in the ‘dark’ after radiation. In this study, bio-based acrylated epoxidized soybean oil (AESO) was cured with UV radiation using radicalic photoinitiator Irgacure 184. Triarylsulphonium hexafluoroantimonate was used as cationic photoinitiator for curing of 3,4-epoxycyclohexylmethyl-3,4-epoxycyclohexanecarboxylate. The effect of curing time and the amount of initiators on the curing degree and thermal properties were investigated. The thermal properties of the coating were analyzed after crosslinking UV irradiation. The level of crosslinking in the coating was evaluated by FTIR analysis. Cationic UV-cured coatings demonstrated excellent adhesion and corrosion resistance properties. Therefore, our study holds a great potential with its simple and low-cost applications.

Keywords: Acrylated epoxidized soybean oil, epoxy carboxylate, thermal properties, UV-curing.

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Authors: Ahmed A. Elshami, Stéphanie Bonnet, Abdelhafid Khelidj

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Corrosion inhibitors are widely used in concrete industry to reduce the corrosion rate of steel rebar which is present in contact with aggressive environments. The present work aims to using Zamzam water from well located within the Masjid al-Haram in Mecca, Saudi Arabia 20 m (66 ft) east of the Kaaba, the holiest place in Islam as corrosion inhibitor for steel in rain water and simulated acid rain. The effect of Zamzam water was investigated by electrochemical impedance spectroscopy (EIS) and Potentiodynamic polarization techniques in Department of Civil Engineering - IUT Saint-Nazaire, Nantes University, France. Zamzam water is considered to be one of the most important steel corrosion inhibitor which is frequently used in different industrial applications. Results showed that zamzam water gave a very good inhibition for steel corrosion in rain water and simulated acid rain.

Keywords: Zamzam water, corrosion inhibitor, rain water and simulated acid rain.

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Authors: Selvakumar Dhanasingh, Shunmuga Kumar Nallaperumal

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Microparticles carrier systems made from naturally occurring polymers based on chitosan/casein system appears to be a promising carrier for the sustained release of orally and parenteral administered drugs. In the current study we followed a microencapsulation technique based aqueous coacervation method to prepare chitosan/casein microparticles of compositions 1:1, 1:2 and 1:5 incorporated with chloramphenicol. Glutaraldehyde was used as a chemical cross-linking agent. The microparticles were prepared by aerosol method and studied by optical microscopy, infrared spectroscopy, thermo gravimetric analysis, swelling studies and drug release studies at various pH. The percentage swelling of the polymers are found to be in the order pH 4 > pH 10 > pH 7 and the increase in casein composition decrease the swelling percentage. The drug release studies also follow the above order.

Keywords: Chitosan/casein micro particles, chloramphenicol, drug release, microencapsulation.

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Authors: M. Sari Yilmaz, N. Karamahmut Mermer

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Coal fly ash is formed as a solid waste product from the combustion of coal in coal fired power stations. Huge amounts of fly ash are produced globally every year and are predicted to increase. Nowadays, less than half of the fly ash is used as a raw material for cement manufacturing, construction and the rest of it is disposed as a waste causing yet another environmental concern. For this reason, the recycling of this kind of slurries into useful materials is quite important in terms of economical and environmental aspects. The purpose of this study is to evaluate the Orhaneli and Tuncbilek coal fly ashes for utilization in some industrial applications. Therefore the mineralogical and chemical compositions of these fly ashes were analyzed by X-ray fluorescence spectroscopy, ourier-transform infrared spectrometer, and X-ray diffraction. The silicon (Si) and aluminum (Al) in the fly ashes were activated by alkali fusion technique with sodium hydroxide. The obtained extracts were analyzed for Si and Al content by inductively coupled plasma optical emission spectrometry.

Keywords: Extraction, Fly ash, Fusion, XRD.

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Authors: M. N. Akhtar, J. N. Akhtar

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The present study evaluates the properties of class F fly ash as a replacement of natural materials in civil engineering construction industry. The low-lime flash similar to class F is the prime variety generated in India, although it has significantly smaller volumes of high-lime fly ash as compared to class C. The chemical and physical characterization of the sample is carried out with the number of experimental approaches in order to investigate all relevant features present in the samples. For chemical analysis, elementary quantitative results from point analysis and scanning electron microscopy (SEM)/dispersive spectroscopy (EDS) techniques were used to identify the element images of different fractions. The physical properties found very close to the range of common soils. Furthermore, the fly ash-based bricks were prepared by the same sample of class F fly ash and the results of compressive strength similar to that of Standard Clay Brick Grade 1 available in the local market of India.

Keywords: Flyash, class F, class C, chemical, physical, SEM, EDS.

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Authors: M.S. Mazăre, A. M. Pană, L. M. Ştefan, M. Silion, M. Bălan, G. Bandur, L. M. Rusnac

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In the last decade, carbohydrates have attracted great attention as renewable resources for the chemical industry. Carbohydrates are abundantly found in nature in the form of monomers, oligomers and polymers, or as components of biopolymers and other naturally occurring substances. As natural products, they play important roles in conferring certain physical, chemical, and biological properties to their carrier molecules.The synthesis of this particular carbohydrate glycomonomer is part of our work to obtain biodegradable polymers. Our current paper describes the synthesis and characterization of a novel carbohydrate glycomonomer starting from D-glucose, in several synthesis steps, that involve the protection/deprotection of the D-glucose ring via acetylation, tritylation, then selective deprotection of the aromaticaliphatic protective group, in order to obtain 1,2,3,4-tetra-O-acetyl- 6-O-allyl-β-D-glucopyranose. The glycomonomer was then obtained by the allylation in drastic conditions of 1,2,3,4-tetra-O-acetyl-6-Oallyl- β-D-glucopyranose with allylic alcohol in the presence of stannic chloride, in methylene chloride, at room temperature. The proposed structure of the glycomonomer, 2,3,4-tri-O-acetyl-1,6-di- O-allyl-β-D-glucopyranose, was confirmed by FTIR, NMR and HPLC-MS spectrometry. This glycomonomer will be further submitted to copolymerization with certain acrylic or methacrylic monomers in order to obtain competitive plastic materials for applications in the biomedical field.

Keywords: allylation, D-glucose, glycomonomer, trityl chloride

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

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Fly ash is an important waste, produced in thermal power plants which causes very important environmental pollutions. For this reason the usage and evaluation the fly ash in various areas are very important. Nearly, 15 million tons/year of fly ash is produced in Turkey. In this study, usage of fly ash with diatomite and molasses for heavy metal (Cd) adsorption from wastewater is investigated. The samples of Seyitomer region fly ash were analyzed by X-ray fluorescence (XRF) and Scanning Electron Microscope (SEM) then diatomite (0 and 1% in terms of fly ash, w/w) and molasses (0-0.75 mL) were pelletized under 30 MPa of pressure for the usage of cadmium (Cd) adsorption in wastewater. After the adsorption process, samples of Seyitomer were analyzed using Optical Emission Spectroscopy (ICP-OES). As a result, it is seen that the usage of Seyitomer fly ash is proper for cadmium (Cd) adsorption and an optimum adsorption yield with 52% is found at a compound with Seyitomer fly ash (10 g), diatomite (0.5 g) and molasses (0.75 mL) at 2.5 h of reaction time, pH:4, 20ºC of reaction temperature and 300 rpm of stirring rate.

Keywords: Heavy metal, fly ash, molasses, diatomite, adsorption, wastewater.

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Authors: Seunghwan Lee

Abstract:

The lubricating properties of commercially available mucins originating from different animal organs, namely bovine submaxillary mucin (BSM) and porcine gastric mucin (PGM), have been characterized at polymeric surfaces for biomedical applications. Atomic force microscopy (AFM) and pin-on-disk tribometry have been employed for tribological studies at nanoscale and macroscale contacts, respectively. Polystyrene (PS) was employed to represent ‘rigid’ contacts, whereas poly(dimethylsiloxane) (PDMS) was employed to represent ‘soft contacts’. To understand the lubricating properties of mucins in correlation with the coverage on surfaces, adsorption properties of mucins onto the polymeric substrates have been characterized by means of optical waveguide light-mode spectroscopy (OWLS). Both mucins showed facile adsorption onto both polymeric substrates, but the lubricity was highly dependent upon the pH change between 2 and 7.

Keywords: Bovine submaxillary mucin (BSM), Porcine Gastric Mucin (PGM), lubricity, biomedical.

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Authors: B.S.Boyanov, M.P.Sandalski, K.I.Ivanov

Abstract:

The production of glass, ceramic materials and many non-ferrous metals (Zn, Cu, Pb, etc.), ferrous metals (pig iron) and others is connected with the use of a considerable number of initial solid raw materials. Before carrying out the basic technological processes (oxidized roasting, melting, agglomeration, baking) it is necessary to mix and homogenize the raw materials that have different chemical and phase content, granulometry and humidity. For this purpose zinc sulfide concentrates differing in origin are studied for their more complete characteristics using chemical, X-ray diffraction analyses, DTA and TGA as well as Mössbauer spectroscopy. The phases established in most concentrates are: β-ZnS, mZnS.nFeS, FeS2, CuFeS2, PbS, SiO2 (α-quartz). With the help of the developed by us a Web-based information system for a continued period of time different mix proportions from zinc concentrates are calculated and used in practice (roasting in fluidized bed reactor), which have to conform to the technological requirements of the zinc hydrometallurgical technological scheme.

Keywords: fluidized bed reactor, roasting, Web-based information system, zinc concentrates.

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Authors: Ravi V. Joat, Pravin S. Bodke, Shradha S. Binani, S. S. Wasnik

Abstract:

A phase diagram of the Ag₂SO₄ - CaSO₄ (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag₂SO₄ + CaSO₄) is observed at 10 mole% CaSO₄ and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca ²⁺ in Ag₂SO₄ is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO₄ content. Amongst other binary compositions, the 80AgSO₄-20CaSO₄ gave improved sinterability/packing density.

Keywords: Ag2SO4-CaSO4 (Silver sulphate–Calcium Sulphate) binaries system, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis).

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Authors: Abhay Kumar Singh

Abstract:

Structural and UV/Visible optical properties can be useful to describe a material for the CIGS solar cell active layer, therefore, this work demonstrates the properties like surface morphology, X-ray Photoelectron Spectroscopy (XPS) bonding energy (EB) core level spectra, UV/Visible absorption spectra, refractive index (n), optical energy band (Eg), reflection spectra for the Cu25 (In16Ga9) Se40Te10 (CIGST-1) and Cu20 (In14Ga9) Se45Te12 (CIGST-2) chalcogenide compositions. Materials have been exhibited homogenous surface morphologies, broading /-or diffusion of bonding energy peaks relative elemental values and a high UV/Visible absorption tendency in the wave length range 400 nm- 850 nm range with the optical energy band gaps 1.37 and 1.42 respectively. Subsequently, UV/Visible reflectivity property in the wave length range 250 nm to 320 nm for these materials has also been discussed.

Keywords: Chalcogen, Optical energy band gap, UV/Visible spectra, XPS spectra.

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Authors: G.Anjali, M.Bhavya, N.Arvind Kumar

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In order to avoid the potentially devastating consequences of global warming and climate change, the carbon dioxide “CO2" emissions caused due to anthropogenic activities must be reduced considerably. This paper presents the first study examining the feasibility of carbon sequestration in construction and demolition “C&D" waste. Experiments were carried out in a self fabricated Batch Reactor at 40ºC, relative humidity of 50-70%, and flow rate of CO2 at 10L/min for 1 hour for water-to-solids ratio of 0.2 to 1.2. The effect of surface area was found by comparing the theoretical extent of carbonation of two different sieve sizes (0.3mm and 2.36mm) of C&D waste. A 38.44% of the theoretical extent of carbonation equating to 4% CO2 sequestration extent was obtained for C&D waste sample for 0.3mm sieve size. Qualitative, quantitative and morphological analyses were done to validate carbonate formation using X-ray diffraction “X.R.D.," thermal gravimetric analysis “T.G.A., “X-Ray Fluorescence Spectroscopy “X.R.F.," and scanning electron microscopy “S.E.M".

Keywords: Alkaline waste, construction and demolition waste, CO2 sequestration, mineral carbonation.

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

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

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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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Authors: Nuridayanti Che Khalib, Kaliyaperumal Thanigaimani, Suhana Arshad, Ibrahim Abdul Razak

Abstract:

The 1:1 cocrystal of 2-amino-4-chloro-6- methylpyrimidine (2A4C6MP) with 4-methylbenzoic acid (4MBA) (I) has been prepared by slow evaporation method in methanol, which was crystallized in monoclinic C2/c space group, Z = 8, and a = 28.431 (2) Å, b = 7.3098 (5) Å, c = 14.2622 (10) Å and β = 109.618 (3)°. The presence of unionized –COOH functional group in cocrystal I was identified both by spectral methods (1H and 13C NMR, FTIR) and X-ray diffraction structural analysis. The 2A4C6MP molecule interact with the carboxylic group of the respective 4MBA molecule through N—H⋯O and O—H⋯N hydrogen bonds, forming a cyclic hydrogen–bonded motif R2 2(8). The crystal structure was stabilized by Npyrimidine—H⋯O=C and C=O—H⋯Npyrimidine types hydrogen bonding interactions. Theoretical investigations have been computed by HF and density function (B3LYP) method with 6–311+G (d,p)basis set. The vibrational frequencies together with 1H and 13C NMR chemical shifts have been calculated on the fully optimized geometry of cocrystal I. Theoretical calculations are in good agreement with the experimental results. Solvent–free formation of this cocrystal I is confirmed by powder X-ray diffraction analysis.

Keywords: Supramolecular Cocrystal, 2-amino-4-chloro-6- methylpyrimidine, Hartree-Fock and DFT Studies, Spectroscopic Analysis.

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Authors: Khawtar Hasan Ahmed, Sasha Omanovic

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

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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: 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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Authors: Salise Oktay, Nilgün Kızılcan, Başak Bengü

Abstract:

At present, formaldehyde-based adhesives such as urea formaldehyde (UF), melamine formaldehyde (MF), melamine-urea formaldehyde (MUF) etc. are mostly used in wood-based panel industry because of their high reactivity, chemical versatility and economic competitiveness. However, formaldehyde-based wood adhesives are produced from non-renewable resources. Hence, there has been a growing interest in the development of environment friendly, economically competitive, bio-based wood adhesives in order to meet wood-based panel industry requirements. In this study, as formaldehyde free adhesive, tannin and starch-based wood adhesive was synthesized. Citric acid and tartaric acid were used as hardener for the resin system. Solid content, viscosity and gel time analyzes of the prepared adhesive were performed in order to evaluate the adhesive processability. FTIR characterization technique was used to elucidate chemical structures of the cured adhesive samples. In order to evaluate the performance of the prepared bio-based resin formulation, particleboards were produced in laboratory scale and mechanical, physical properties of the boards were investigated. Besides, formaldehyde contents of the boards were determined by using perforator method. The obtained results revealed that the developed bio-based wood adhesive formulation can be a good potential candidate to use in wood-based panel industry with some developments.

Keywords: Wood adhesive, cornstarch, mimosa tannin, particleboard.

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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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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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