Search results for: Raman spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 397

Search results for: Raman spectroscopy

97 Investigating the Geopolymerization Process of Aluminosilicates and Its Impact on the Compressive Strength of the Produced Geopolymers

Authors: Heba Z. Fouad, Tarek M. Madkour, Safwan A. Khedr

Abstract:

This paper investigates multiple factors that impact the formation of geopolymers and their compressive strength to be utilized in construction as an environmentally-friendly material. Bentonite and Kaolinite were thermally calcinated at 750 °C to obtain Metabentonite and Metakaolinite with higher reactivity. Both source materials were activated using a solution of sodium hydroxide (NaOH). Thereafter, samples were cured at different temperatures. The samples were analyzed chemically using a host of spectroscopic techniques. The bulk density and compressive strength of the produced geopolymer pastes were studied. Findings indicate that the ratio of NaOH solution to source material affects the compressive strength, being optimal at 0.54. Moreover, controlled heat curing was proven effective to improve compressive strength. The existence of characteristic Fourier Transform Infrared Spectroscopy (FTIR) peaks at approximately 1020 cm-1 and 460 cm-1 which correspond to the asymmetric stretching vibration of Si-O-T and bending vibration of Si-O-Si, hence, confirming the formation of the target geopolymer.

Keywords: alcination of metakaolinite, compressive strength, FTIR analysis, geopolymer, green cement

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96 The Mechanistic and Oxidative Study of Methomyl and Parathion Degradation by Fenton Process

Authors: Chihhao Fan, Ming-Chu Liao

Abstract:

The purpose of this study is to investigate the chemical degradation of the organophosphorus pesticide of parathion and carbamate insecticide of methomyl in the aqueous phase through Fenton process. With the employment of batch Fenton process, the degradation of the two selected pesticides at different pH, initial concentration, humic acid concentration, and Fenton reagent dosages was explored. The Fenton process was found effective to degrade parathion and methomyl. The optimal dosage of Fenton reagents (i.e., molar concentration ratio of H2O2 to Fe2+) at pH 7 for parathion degradation was equal to 3, which resulted in 50% removal of parathion. Similarly, the optimal dosage for methomyl degradation was 1, resulting in 80% removal of methomyl. This study also found that the presence of humic substances has enhanced pesticide degradation by Fenton process significantly. The mass spectroscopy results showed that the hydroxyl free radical may attack the single bonds with least energy of investigated pesticides to form smaller molecules which is more easily to degrade either through physio-chemical or bilolgical processes.

Keywords: Fenton Process, humic acid, methomyl, parathion, pesticides

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95 Langmuir–Blodgett Films of Polyaniline for Efficient Detection of Uric Acid

Authors: Kashima Arora, Monika Tomar, Vinay Gupta

Abstract:

Langmuir–Blodgett (LB) films of polyaniline (PANI) grown onto ITO coated glass substrates were utilized for the fabrication of Uric acid biosensor for efficient detection of uric acid by immobilizing Uricase via EDC–NHS coupling. The modified electrodes were characterized by atomic force microscopy (AFM). The response characteristics after immobilization of uricase were studied using cyclic voltammetry and electrochemical impedance spectroscopy techniques. The uricase/PANI/ITO/glass bioelectrode studied by CV and EIS techniques revealed detection of uric acid in a wide range of 0.05 mM to 1.0 mM, covering the physiological range in blood. A low Michaelis–Menten constant (Km) of 0.21 mM indicates the higher affinity of immobilized Uricase towards its analyte (uric acid). The fabricated uric acid biosensor based on PANI LB films exhibits excellent sensitivity of 0.21 mA/mM with a response time of 4 s, good reproducibility, long shelf life (8 weeks) and high selectivity.

Keywords: Uric acid; biosensor, PANI, Langmuir Blodgett films deposition.

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94 Surface Roughness Evaluation for EDM of En31 with Cu-Cr-Ni Powder Metallurgy Tool

Authors: Amoljit S. Gill, Sanjeev Kumar

Abstract:

In this study, Electrical Discharge Machining (EDM) is used to modify the surface of high carbon steel En31 with the help of tool electrode (Copper-Chromium-Nickel) manufactured by powder metallurgy (PM) process. The effect of EDM on surface roughness during surface alloying is studied. Taguchi’s Design of experiment (DOE) and L18 orthogonal array is used to find the best level of input parameters in order to achieve high surface finish. Six input parameters are considered and their percentage contribution towards surface roughness is investigated by analysis of variances (ANOVA). Experimental results show that an hard alloyed surface (1.21% carbon, 2.14% chromium and 1.38% nickel) with surface roughness of 3.19µm can be generated using EDM with PM tool. Additionally, techniques like Scanning Electron Microscope (SEM) and Energy Dispersive Spectroscopy (EDS) are used to analyze the machined surface and EDMed layer composition, respectively. The increase in machined surface micro-hardness (101%) may be related to the formation of carbides containing chromium.

Keywords: Electrical Discharge Machining, Surface Roughness, Powder metallurgy compact tools, Taguchi DOE technique.

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93 The Effect of Waste Magnesium to Boric Acid Ratio in Hydrothermal Magnesium Borate Synthesis at 70oC

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

Abstract:

Magnesium wastes are produced by many industrial activities. This waste problem is becoming a future problem for the world. Magnesium borates have many advantages such as; high corrosion resistance, heat resistance, high coefficient of elasticity and can also be used in the production of material against radiation. Addition, magnesium borates have great potential in sectors including ceramic and detergents industry and superconducting materials. In this study, using the starting materials of waste magnesium and H3BO3 the hydrothermal method was applied at a moderate temperature of 70oC. Several mole ratios of waste magnesium to H3BO3 are selected as; 1:2, 1:4, 1:6, 1:8, 1:10. Reaction time was determined as 1 hour. After the synthesis, X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are applied to products. As a result the forms of mcallisterite “Mg2(B6O7(OH)6)2.9(H2O)”, admontite “MgO(B2O3)3.7(H2O)” and magnesium boron hydrate (MgO(B2O3)3.6(H2O)” are obtained. 

Keywords: Hydrothermal synthesis, magnesium borates, waste magnesium.

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92 A Study on Removal of Toluidine Blue Dye from Aqueous Solution by Adsorption onto Neem Leaf Powder

Authors: Himanshu Patel, R. T. Vashi

Abstract:

Adsorption of Toluidine blue dye from aqueous solutions onto Neem Leaf Powder (NLP) has been investigated. The surface characterization of this natural material was examined by Particle size analysis, Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and X-Ray Diffraction (XRD). The effects of process parameters such as initial concentration, pH, temperature and contact duration on the adsorption capacities have been evaluated, in which pH has been found to be most effective parameter among all. The data were analyzed using the Langmuir and Freundlich for explaining the equilibrium characteristics of adsorption. And kinetic models like pseudo first- order, second-order model and Elovich equation were utilized to describe the kinetic data. The experimental data were well fitted with Langmuir adsorption isotherm model and pseudo second order kinetic model. The thermodynamic parameters, such as Free energy of adsorption (AG"), enthalpy change (AH') and entropy change (AS°) were also determined and evaluated.

Keywords: Adsorption, isotherm models, kinetic models, temperature, toluidine blue dye, surface chemistry.

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91 Identification and Characterization of Heavy Metal Resistant Bacteria from the Klip River

Authors: P. Chihomvu, P. Stegmann, M. Pillay

Abstract:

Pollution of the Klip River has caused microorganisms inhabiting it to develop protective survival mechanisms. This study isolated and characterized the heavy metal resistant bacteria in the Klip River. Water and sediment samples were collected from six sites along the course of the river. The pH, turbidity, salinity, temperature and dissolved oxygen were measured in-situ. The concentrations of six heavy metals (Cd, Cu, Fe, Ni, Pb and Zn) of the water samples were determined by atomic absorption spectroscopy. Biochemical and antibiotic profiles of the isolates were assessed using the API 20E® and Kirby Bauer Method. Growth studies were carried out using spectrophotometric methods. The isolates were identified using 16SrDNA sequencing. The uppermost part of the Klip River with the lowest pH had the highest levels of heavy metals. Turbidity, salinity and specific conductivity increased measurably at Site 4 (Henley on Klip Weir). MIC tests showed that 16 isolates exhibited high iron and lead resistance. Antibiotic susceptibility tests revealed that the isolates exhibited multitolerances to drugs such as Tetracycline, Ampicillin, and Amoxicillin.

Keywords: Klip River, heavy metals, resistance.

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90 Study of the Transport of Multivalent Metal Cations through Cation-Exchange Membranes by Electrochemical Impedance Spectroscopy

Authors: V. Pérez-Herranz, M. Pinel, E. M. Ortega, M. García-Gabaldón

Abstract:

In the present work, Electrochemical Impedance Spectrocopy (EIS) is applied to study the transport of different metal cations through a cation-exchange membrane. This technique enables the identification of the ionic-transport characteristics and to distinguish between different transport mechanisms occurring at different current density ranges. The impedance spectra are dependent on the applied dc current density, on the type of cation and on the concentration. When the applied dc current density increases, the diameter of the impedance spectra loops increases because all the components of membrane system resistance increase. The diameter of the impedance plots decreases in the order of Na(I), Ni(II) and Cr(III) due to the increased interactions between the negatively charged sulfonic groups of the membrane and the cations with greater charge. Nyquist plots are shifted towards lower values of the real impedance, and its diameter decreases with the increase of concentration due to the decrease of the solution resistance.

Keywords: Ion-exchange Membranes, Electrochemical Impedance Espectroscopy, Multivalent Metal Cations.

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89 The Extension of Monomeric Computational Results to Polymeric Measurable Properties: An Introductory Computational Chemistry Experiment

Authors: Zhao Jing, Bai Yongqing, Shi Qiaofang, Zang Yang, Zhang Huaihao

Abstract:

Advances in software technology enable the computational chemistry to be commonly applied in various research fields, especially in pedagogy. Thus, in order to expand and improve experimental instructions of computational chemistry for undergraduates, we designed an introductory experiment—research on acrylamide molecular structure and physicochemical properties. Initially, students construct molecular models of acrylamide and polyacrylamide in Gaussian and Materials Studio software respectively. Then, the infrared spectral data, atomic charge and molecular orbitals of acrylamide as well as solvation effect of polyacrylamide are calculated to predict their physicochemical performance. At last, rheological experiments are used to validate these predictions. Through the combination of molecular simulation (performed on Gaussian, Materials Studio) with experimental verification (rheology experiment), learners have deeply comprehended the chemical nature of acrylamide and polyacrylamide, achieving good learning outcomes.

Keywords: Upper-division undergraduate, computer-based learning, laboratory instruction, amides, molecular modeling, spectroscopy.

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88 Natural Radioactivity in Foods Consumed in Turkey

Authors: E. Kam, G. Karahan, H. Aslıyuksek, A. Bozkurt

Abstract:

This study aims to determine the natural radioactivity levels in some foodstuffs produced in Turkey. For this purpose, 48 different foods samples were collected from different land parcels throughout the country. All samples were analyzed to designate both gross alpha and gross beta radioactivities and the radionuclides’ concentrations. The gross alpha radioactivities were measured as below 1 Bq kg-1 in most of the samples, some of them being due to the detection limit of the counting system. The gross beta radioactivity levels ranged from 1.8 Bq kg-1 to 453 Bq kg-1, larger levels being observed in leguminous seeds while the highest level being in haricot bean. The concentrations of natural radionuclides in the foodstuffs were investigated by the method of gamma spectroscopy. High levels of 40K were measured in all the samples, the highest activities being again in leguminous seeds. Low concentrations of 238U and 226Ra were found in some of the samples, which are comparable to the reported results in the literature. Based on the activity concentrations obtained in this study, average annual effective dose equivalents for the radionuclides 226Ra, 238U, and 40K were calculated as 77.416 µSv y-1, 0.978 µSv y-1, and 140.55 µSv y-1, respectively.

Keywords: Foods, radioactivity, gross alpha, gross beta, annual equivalent dose, Turkey.

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87 Fabrication and Characterization of CdS Nanoparticles Annealed by using Different Radiations

Authors: Aneeqa Sabah, Saadat Anwar Siddiqi, Salamat Ali

Abstract:

The systematic manipulations of shapes and sizes of inorganic compounds greatly benefit the various application fields including optics, magnetic, electronics, catalysis and medicine. However shape control has been much more difficult to achieve. Hence exploration of novel method for the preparation of differently shaped nanoparticles is challenging research area. II-VI group of semiconductor cadmium sulphide (CdS) nanostructure with different morphologies (such as, acicular like, mesoporous, spherical shapes) and of crystallite sizes vary from 11 to 16 nm were successfully synthesized by chemical aqueous precipitation of Cd2+ ions with homogeneously released S2- ions from decomposition of cadmium sulphate (CdSO4) and thioacetamide (CH3CSNH2) by annealing at different radiations (microwave, ultrasonic and sunlight) with matter and systematic research has been done for various factors affecting the controlled growth rate of CdS nanoparticles. The obtained nanomaterials have been characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravometric (DSC-TGA) analysis and Scanning Electron Microscopy (SEM). The result indicates that on increasing the reaction time particle size increases but on increasing the molar ratios grain size decreases.

Keywords: CdS nanoparticles, Morphology, Oxidation, Radiations

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86 Development of a Porous Silica Film by Sol-gel Process

Authors: Binay K. Dutta, Tayseir M. Abd Ellateif, Saikat Maitra

Abstract:

In the present work homogeneous silica film on silicon was fabricated by colloidal silica sol. The silica sol precursor with uniformly granular particle was derived by the alkaline hydrolysis of tetraethoxyorthosilicate (TEOS) in presence of glycerol template. The film was prepared by dip coating process. The templated hetero-structured silica film was annealed at elevated temperatures to generate nano- and meso porosity in the film. The film was subsequently annealed at different temperatures to make it defect free and abrasion resistant. The sol and the film were characterized by the measurement of particle size distribution, scanning electron microscopy, XRD, FTIR spectroscopy, transmission electron microscopy, atomic force microscopy, measurement of the refractive index, thermal conductivity and abrasion resistance. The porosity of the films decreased whereas refractive index and dielectric constant of it `increased with the increase in the annealing temperature. The thermal conductivity of the films increased with the increase in the film thickness. The developed porous silica film holds strong potential for use in different areas.

Keywords: Silica film, Nanoporous, Sol-gel, Templating, Dip coating.

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85 Experimental Investigation on Effect of the Zirconium + Magnesium Coating of the Piston and Valve of the Single-Cylinder Diesel Engine to the Engine Performance and Emission

Authors: Erdinç Vural, Bülent Özdalyan, Serkan Özel

Abstract:

The four-stroke single cylinder diesel engine has been used in this study, the pistons and valves of the engine have been stabilized, the aluminum oxide (Al2O3) in different ratios has been added in the power of zirconium (ZrO2) magnesium oxide (MgO), and has been coated with the plasma spray method. The pistons and valves of the combustion chamber of the engine are coated with 5 different (ZrO2 + MgO), (ZrO2 + MgO + 25% Al2O3), (ZrO2 + MgO + 50% Al2O3), (ZrO2 + MgO + 75% Al2O3), (Al2O3) sample. The material tests have been made for each of the coated engine parts with the scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) using Cu Kα radiation surface analysis methods. The engine tests have been repeated for each sample in any electric dynamometer in full power 1600 rpm, 2000 rpm, 2400 rpm and 2800 rpm engine speeds. The material analysis and engine tests have shown that the best performance has been performed with (ZrO2 + MgO + 50% Al2O3). Thus, there is no significant change in HC and Smoke emissions, but NOx emission is increased, as the engine improves power, torque, specific fuel consumption and CO emissions in the tests made with sample A3.

Keywords: Ceramic coating, material characterization, engine performance, exhaust emissions.

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84 Gamma Irradiation Effect on Structural and Optical Properties of Bismuth-Boro-Tellurite Glasses

Authors: A. Azuraida, M. K. Halimah, C. A. C. Azurahanim, M. Ishak

Abstract:

The changes of the optical and structural properties of Bismuth-Boro-Tellurite glasses pre and post gamma irradiation were studied. Six glass samples, with different composition [(TeO2)0.7 (B2O3)0.3]1-x (Bi2O3)x prepared by melt quenching method were irradiated with 25kGy gamma radiation at room temperature. The Fourier Transform Infrared Spectroscopy (FTIR) was used to explore the structural bonding in the prepared glass samples due to exposure, while UV-VIS Spectrophotometer was used to evaluate the changes in the optical properties before and after irradiation. Gamma irradiation causes profound changes in the peak intensity as shown by FTIR spectra which is due to the breaking of the network bonding. Before gamma irradiation, the optical band gap, Eg value decreased from 2.44 eV to 2.15 eV with the addition of Bismuth content. The value kept decreasing (from 2.18 eV to 2.00 eV) following exposure to gamma radiation due to the increase of non-bridging oxygen (NBO) and the increase of defect in the glass. In conclusion, the glass with high content of Bi2O3 (0.30Bi) give smallest Eg and show less changes in FTIR spectra after gamma irradiation which indicate that this glass is more resistant to gamma radiation compared to other glasses.

Keywords: Boro-Tellurite, bismuth, gamma radiation, optical properties.

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83 Nanocharacterization of PIII Treated 7075 Aluminum Alloy

Authors: Bruno Bacci Fernandes, Stephan Mändl, Ataíde Ribeiro da Silva Junior, José Osvaldo Rossi, Mário Ueda

Abstract:

Nitrogen implantation in aluminum and its alloys is acquainted for the difficulties in obtaining modified layers deeper than 200 nm. The present work addresses a new method to overcome such a problem; although, the coating with nitrogen and oxygen obtained by plasma immersion ion implantation (PIII) into a 7075 aluminum alloy surface was too shallow. This alloy is commonly used for structural parts in aerospace applications. Such a layer was characterized by secondary ion mass spectroscopy, electron microscopy, and nanoindentation experiments reciprocating wear tests. From the results, one can assume that the wear of this aluminum alloy starts presenting severe abrasive wear followed by an additional adhesive mechanism. PIII produced a slight difference, as shown in all characterizations carried out in this work. The results shown here can be used as the scientific basis for further nitrogen PIII experiments in aluminum alloys which have the goal to produce thicker modified layers or to improve their surface properties.

Keywords: Aluminum alloys, plasma immersion ion implantation, tribological properties, hardness, nanofatigue.

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82 Functionalization of Polypropylene with Chiral Monomer for Improving Hemocompatibility

Authors: Xiaodong Xu, Dan Zhao, Xiujuan Chang, Chunming Li, Huiyun Zhou, Xin Li, Qiang Shi, Shifang Luan, Jinghua Yin

Abstract:

Polypropylene (PP) is one of the most commonly used plastics because of its low density, outstanding mechanical properties, and low cost. However, its drawbacks such as low surface energy, poor dyeability, lack of chemical functionalities, and poor compatibility with polar polymers and inorganic materials, have restricted the application of PP. To expand its application in biomedical materials, functionalization is considered to be the most effective way. In this study, PP was functionalized with a chiral monomer, (S)-1-acryloylpyrrolidine-2-carboxylic acid ((S)-APCA), by free-radical grafting in the solid phase. The grafting degree of PP-g-APCA was determined by chemical titration method, and the chemical structure of functionalized PP was characterized by FTIR spectroscopy, which confirmed that the chiral monomer (S)-APCA was successfully grafted onto PP. Static water contact angle results suggested that the surface hydrophilicity of PP was significantly improved by solid phase grafting and assistance of surface water treatment. Protein adsorption and platelet adhesion results showed that hemocompatibility of PP was greatly improved by grafting the chiral monomer.

Keywords: Functionalization, polypropylene, chiral monomer, hemocompatibility.

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81 Performance Enhancement of Dye-Sensitized Solar Cells by MgO Coating on TiO2 Electrodes

Authors: C. Photiphitak, P. Rakkwamsuk, P. Muthitamongkol, C. Thanachayanont

Abstract:

TiO2/MgO composite films were prepared by coating the magnesium acetate solution in the pores of mesoporous TiO2 films using a dip coating method. Concentrations of magnesium acetate solution were varied in a range of 1x10-4 – 1x10-1 M. The TiO2/MgO composite films were characterized by scanning electron microscopy (SEM), transmission electron microscropy (TEM), electrochemical impedance spectroscopy(EIS) , transient voltage decay and I-V test. The TiO2 films and TiO2/MgO composite films were immersed in a 0.3 mM N719 dye solution. The Dye-sensitized solar cells with the TiO2/MgO/N719 structure showed an optimal concentration of magnesium acetate solution of 1x10-3 M resulting in the MgO film estimated thickness of 0.0963 nm and giving the maximum efficiency of 4.85%. The improved efficiency of dyesensitized solar cell was due to the magnesium oxide film as the wide band gap coating decays the electron back transfer to the triiodide electrolyte and reduce charge recombination.

Keywords: Magnesium oxide thin film, TiO2/MgO composite films, Electrochemical Impedance Spectrum, Transient voltage decay

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80 Thermosensitive Hydrogel Development for Its Possible Application in Cardiac Cell Therapy

Authors: Lina Paola Orozco-Marín, Yuliet Montoya, John Bustamante

Abstract:

Ischemic events can culminate in acute myocardial infarction with irreversible cardiac lesions that cannot be restored due to the limited regenerative capacity of the heart. Tissue engineering proposes therapeutic alternatives by using biomaterials to resemble the native extracellular medium combined with healthy and functional cells. This research focused on developing a natural thermosensitive hydrogel, its physical-chemical characterization and in vitro biocompatibility determination. Hydrogels’ morphological characterization was carried out through scanning electron microscopy and its chemical characterization by employing Infrared Spectroscopy technic. In addition, the biocompatibility was determined using fetal human ventricular cardiomyocytes cell line RL-14 and the MTT cytotoxicity test according to the ISO 10993-5 standard. Four biocompatible and thermosensitive hydrogels were obtained with a three-dimensional internal structure and two gelation times. The results show the potential of the hydrogel to increase the cell survival rate to the cardiac cell therapies under investigation and lay the foundations to continue with its characterization and biological evaluation both in vitro and in vivo models.

Keywords: cardiac cell therapy, cardiac ischemia, natural polymers, thermosensitive hydrogel

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79 Fracture Toughness Properties and FTIR Analysis of Corn Fiber Green Composites

Authors: Ahmed Mudhafar Hashim, Aseel Mahmood Abdullah

Abstract:

The present work introduced a green composite consisting of corn natural fiber of constant concentration of 10% by weight incorporation with poly methyl methacrylate matrix biomaterial prepared by hand lay-up technique. Corn natural fibers were treated with two concentrations of sodium hydroxide solution (3% and 5%) with different immersed time (1.5 and 3 hours) at room temperature. The fracture toughness test of untreated and alkali treated corn fiber composites were performed. The effect of chemically treated on fracture properties of composites has been analyzed using Fourier transform infrared (FTIR) spectroscopy. The experimental results showed that the alkali treatment improved the fracture properties in terms of plane strain fracture toughness KIC. It was found that the plane strain fracture toughness KIC increased by up to 62% compared to untreated fiber composites. On the other hand, increases in both concentrations of alkali solution and time of soaking to 5% NaOH and 3 hours, respectively reduced the values of KIC lower than the value of the unfilled material.

Keywords: green composites, fracture toughness, corn natural fiber, Bio-PMMA

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78 Artificial Accelerated Ageing Test of 22 kVXLPE Cable for Distribution System Applications in Thailand

Authors: A. Rawangpai, B. Maraungsri, N. Chomnawang

Abstract:

This paper presents the experimental results on artificial ageing test of 22 kV XLPE cable for distribution system application in Thailand. XLPE insulating material of 22 kV cable was sliced to 60-70 μm in thick and was subjected to ac high voltage at 23 Ôùª C, 60 Ôùª C and 75 Ôùª C. Testing voltage was constantly applied to the specimen until breakdown. Breakdown voltage and time to breakdown were used to evaluate life time of insulating material. Furthermore, the physical model by J. P. Crine for predicts life time of XLPE insulating material was adopted as life time model and was calculated in order to compare the experimental results. Acceptable life time results were obtained from Crine-s model comparing with the experimental result. In addition, fourier transform infrared spectroscopy (FTIR) for chemical analysis and scanning electron microscope (SEM) for physical analysis were conducted on tested specimens.

Keywords: Artificial accelerated ageing test, XLPE cable, distribution system, insulating material, life time, life time model

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77 Novel NMR-Technology to Assess Food Quality and Safety

Authors: Markus Link, Manfred Spraul, Hartmut Schaefer, Fang Fang, Birk Schuetz

Abstract:

High Resolution NMR Spectroscopy offers unique screening capabilities for food quality and safety by combining non-targeted and targeted screening in one analysis.

The objective is to demonstrate, that due to its extreme reproducibility NMR can detect smallest changes in concentrations of many components in a mixture, which is best monitored by statistical evaluation however also delivers reliable quantification results.

The methodology typically uses a 400 MHz high resolution instrument under full automation after minimized sample preparation.

For example one fruit juice analysis in a push button operation takes at maximum 15 minutes and delivers a multitude of results, which are automatically summarized in a PDF report.

The method has been proven on fruit juices, where so far unknown frauds could be detected. In addition conventional targeted parameters are obtained in the same analysis. This technology has the advantage that NMR is completely quantitative and concentration calibration only has to be done once for all compounds. Since NMR is so reproducible, it is also transferable between different instruments (with same field strength) and laboratories. Based on strict SOP`s, statistical models developed once can be used on multiple instruments and strategies for compound identification and quantification are applicable as well across labs.

Keywords: Automated solution, NMR, non-targeted screening, targeted screening.

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76 Enhancing Protein Incorporation in Calcium Phosphate Coating on Titanium by Rapid Biomimetic Co-Precipitation Technique

Authors: J. Suwanprateeb, F. Thammarakcharoen

Abstract:

Calcium phosphate coating (CaP) has been employed for protein delivery, but the typical direct protein adsorption on the coating led to low incorporation content and fast release of the protein from the coating. By using bovine serum albumin (BSA) as a model protein, rapid biomimetic co-precipitation between calcium phosphate and BSA was employed to control the distribution of BSA within calcium phosphate coating during biomimetic formation on titanium surface for only 6 h at 50oC in an accelerated calcium phosphate solution. As a result, the amount of BSA incorporation and release duration could be increased by using a rapid biomimetic coprecipitation technique. Up to 43 fold increases in the BSA incorporation content and the increase from 6 h to more than 360 h in release duration compared to typical direct adsorption technique were observed depending on the initial BSA concentration used during coprecipitation (1, 10 and 100 μg.ml-1). From x-ray diffraction and Fourier transform infrared spectroscopy studies, the coating composition was not altered with the incorporation of BSA by this rapid biomimetic co-precipitation and mainly comprised octacalcium phosphate and hydroxyapatite. However, the microstructure of calcium phosphate crystals changed from straight, plate-like units to curved, plate-like units with increasing BSA content.

Keywords: Biomimetic, Calcium Phosphate Coating, Protein, Titanium.

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75 Microstructural and Electrochemical Investigation of Carbon Coated Nanograined LiFePO4 as Cathode Material for Li-Batteries

Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

Abstract:

Lithium iron phosphate (LiFePO4) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO4 (LFP) and carbon-coated nanograined LiFePO4 (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: Ceramics, microstructure, electrochemical measurements, energy storage, transmission electron microscope.

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74 Characterization and Detection of Cadmium Ion Using Modification Calixarene with Multiwalled Carbon Nanotubes

Authors: Amira Shakila Razali, Faridah Lisa Supian, Muhammad Mat Salleh, Suraini Abu Bakar

Abstract:

Water contamination by toxic compound is one of the serious environmental problems today. These toxic compounds mostly originated from industrial effluents, agriculture, natural sources and human waste. These studies focus on modification of multiwalled carbon nanotube (MWCNTs) with nanoparticle of calixarene and explore the possibility of using this modification for the remediation of cadmium in water. The nanocomposites were prepared by dissolving calixarene in chloroform solution as solvent, followed by additional multiwalled carbon nanotube (MWCNTs) then sonication process for 3 hour and fabricated the nanocomposites on substrate by spin coating method. Finally, the nanocomposites were tested on cadmium ion (10 mg/ml). The morphology of nanocomposites was investigated by FESEM showing the formation of calixarene on the outer walls of carbon nanotube and cadmium ion also clearly seen from the micrograph. This formation was supported by using energy dispersive x-ray (EDX). The presence of cadmium ions in the films, leads to some changes in the surface potential and Fourier Transform Infrared spectroscopy (FTIR).The nanocomposites MWCNTs-calixarene have potential for development of sensor for pollutant monitoring and nanoelectronics devices applications.

Keywords: Calixarene, Multiwalled Carbon Nanotubes, Cadmium, Surface Potential.

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73 Off-Line Detection of “Pannon Wheat” Milling Fractions by Near-Infrared Spectroscopic Methods

Authors: E. Izsó, M. Bartalné-Berceli, Sz. Gergely, A. Salgó

Abstract:

The aim of this investigation is to elaborate nearinfrared methods for testing and recognition of chemical components and quality in “Pannon wheat” allied (i.e. true to variety or variety identified) milling fractions as well as to develop spectroscopic methods following the milling processes and evaluate the stability of the milling technology by different types of milling products and according to sampling times, respectively. These wheat categories produced under industrial conditions where samples were collected versus sampling time and maximum or minimum yields. The changes of the main chemical components (such as starch, protein, lipid) and physical properties of fractions (particle size) were analysed by dispersive spectrophotometers using visible (VIS) and near-infrared (NIR) regions of the electromagnetic radiation. Close correlation were obtained between the data of spectroscopic measurement techniques processed by various chemometric methods (e.g. principal component analysis [PCA], cluster analysis [CA]) and operation condition of milling technology. It is obvious that NIR methods are able to detect the deviation of the yield parameters and differences of the sampling times by a wide variety of fractions, respectively. NIR technology can be used in the sensitive monitoring of milling technology.

Keywords: Allied wheat fractions, CA, milling process, nearinfrared spectroscopy, PCA.

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72 Beijerinckia indica Extracellular Extract Mediated Green Synthesis of Silver Nanoparticles with Antioxidant and Antibacterial Activities against Clinical Pathogens

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

Abstract:

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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71 Synthesis and Characterization of Nickel and Sulphur Sensitized Zinc Oxide Structures

Authors: Ella C. Linganiso, Bonex W. Mwakikunga, Trilock Singh, Sanjay Mathur, Odireleng M. Ntwaeaborwa

Abstract:

The use of nanostructured semiconducting material to catalyze degradation of environmental pollutants still receives much attention to date. One of the desired characteristics for pollutant degradation under ultra-violet visible light is the materials with extended carrier charge separation that allows for electronic transfer between the catalyst and the pollutants. In this work, zinc oxide n-type semiconductor vertically aligned structures were fabricated on silicon (100) substrates using the chemical bath deposition method. The as-synthesized structures were treated with nickel and sulphur. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy were used to characterize the phase purity, structural dimensions and elemental composition of the obtained structures respectively. Photoluminescence emission measurements showed a decrease in both the near band edge emission as well as the defect band emission upon addition of nickel and sulphur with different concentrations. This was attributed to increased charger-carrier-separation due to the presence of Ni-S material on ZnO surface, which is linked to improved charge transfer during photocatalytic reactions.

Keywords: Carrier-charge-separation, nickel, sulphur, zinc oxide, photoluminescence.

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70 Conversion of Jatropha curcas Oil to Ester Biolubricant Using Solid Catalyst Derived from Saltwater Clam Shell Waste (SCSW)

Authors: Said Nurdin, Fatimah A. Misebah, Rosli M. Yunus, Mohd S. Mahmud, Ahmad Z. Sulaiman

Abstract:

The discarded clam shell waste, fossil and edible oil as biolubricant feedstocks create environmental impacts and food chain dilemma, thus this work aims to circumvent these issues by using activated saltwater clam shell waste (SCSW) as solid catalyst for conversion of Jatropha curcas oil as non-edible sources to ester biolubricant. The characterization of solid catalyst was done by Differential Thermal Analysis-Thermo Gravimetric Analysis (DTATGA), X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Field Emission Scanning Electron Microscopy (FESEM) and Fourier Transformed Infrared Spectroscopy (FTIR) analysis. The calcined catalyst was used in the transesterification of Jatropha oil to methyl ester as the first step, and the second stage was involved the reaction of Jatropha methyl ester (JME) with trimethylolpropane (TMP) based on the various process parameters. The formated biolubricant was analyzed using the capillary column (DB-5HT) equipped Gas Chromatography (GC). The conversion results of Jatropha oil to ester biolubricant can be found nearly 96.66%, and the maximum distribution composition mainly contains 72.3% of triester (TE).

Keywords: Conversion, ester biolubricant, Jatropha curcas oil, solid catalyst.

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69 Cadmium Filter Cake of a Hydrometallurgical Zinc Smelter as a New Source for the Biological Synthesis of CdS Quantum Dots

Authors: Mehran Bakhshi, Mohammad Raouf Hosseini, Mohammadhosein Rahimi

Abstract:

The cadmium sulfide nanoparticles were synthesized from the nickel-cadmium cake of a hydrometallurgical zinc producing plant and sodium sulfide as Cd2+ and S-2 sources, respectively. Also, the synthesis process was performed by using the secretions of Bacillus licheniformis as bio-surfactant. Initially, in order to obtain a cadmium rich solution, two following steps were carried out: 1) Alkaline leaching for the removal of zinc oxide from the cake, and 2) acidic leaching to dissolve cadmium from the remained solid residue. Afterward, the obtained CdSO4 solution was used for the nanoparticle biosynthesis. Nanoparticles were characterized by the energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) to confirm the formation of CdS crystals with cubic structure. Also, transmission electron microscopy (TEM) was applied to determine the particle sizes which were in 2-10 nm range. Moreover, the presence of the protein containing bio-surfactants was approved by using infrared analysis (FTIR). In addition, the absorbance below 400 nm confirms quantum particles’ size. Finally, it was shown that valuable CdS quantum dots could be obtained from the industrial waste products via environment-friendly biological approaches.

Keywords: Biosynthesis, cadmium cake, cadmium sulfide, nanoparticle, zinc smelter.

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68 Investigation on Polymer Based Nano-Silver as Food Packaging Materials

Authors: A. M. Metak, T. T. Ajaal

Abstract:

Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO2) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO2 nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO2 nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based upon the relevant European safety Directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO2 nanoparticles into the selected food matrices.

Keywords: Nano-silver, antimicrobial food packaging, migration, titanium dioxide.

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