Search results for: electrochemical impedence spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 2461

Search results for: electrochemical impedence spectroscopy

1201 Deasphalting of Crude Oil by Extraction Method

Authors: A. N. Kurbanova, G. K. Sugurbekova, N. K. Akhmetov

Abstract:

The asphaltenes are heavy fraction of crude oil. Asphaltenes on oilfield is known for its ability to plug wells, surface equipment and pores of the geologic formations. The present research is devoted to the deasphalting of crude oil as the initial stage refining oil. Solvent deasphalting was conducted by extraction with organic solvents (cyclohexane, carbon tetrachloride, chloroform). Analysis of availability of metals was conducted by ICP-MS and spectral feature at deasphalting was achieved by FTIR. High contents of asphaltenes in crude oil reduce the efficiency of refining processes. Moreover, high distribution heteroatoms (e.g., S, N) were also suggested in asphaltenes cause some problems: environmental pollution, corrosion and poisoning of the catalyst. The main objective of this work is to study the effect of deasphalting process crude oil to improve its properties and improving the efficiency of recycling processes. Experiments of solvent extraction are using organic solvents held in the crude oil JSC “Pavlodar Oil Chemistry Refinery. Experimental results show that deasphalting process also leads to decrease Ni, V in the composition of the oil. One solution to the problem of cleaning oils from metals, hydrogen sulfide and mercaptan is absorption with chemical reagents directly in oil residue and production due to the fact that asphalt and resinous substance degrade operational properties of oils and reduce the effectiveness of selective refining of oils. Deasphalting of crude oil is necessary to separate the light fraction from heavy metallic asphaltenes part of crude oil. For this oil is pretreated deasphalting, because asphaltenes tend to form coke or consume large quantities of hydrogen. Removing asphaltenes leads to partly demetallization, i.e. for removal of asphaltenes V/Ni and organic compounds with heteroatoms. Intramolecular complexes are relatively well researched on the example of porphyinous complex (VO2) and nickel (Ni). As a result of studies of V/Ni by ICP MS method were determined the effect of different solvents-deasphalting – on the process of extracting metals on deasphalting stage and select the best organic solvent. Thus, as the best DAO proved cyclohexane (C6H12), which as a result of ICP MS retrieves V-51.2%, Ni-66.4%? Also in this paper presents the results of a study of physical and chemical properties and spectral characteristics of oil on FTIR with a view to establishing its hydrocarbon composition. Obtained by using IR-spectroscopy method information about the specifics of the whole oil give provisional physical, chemical characteristics. They can be useful in the consideration of issues of origin and geochemical conditions of accumulation of oil, as well as some technological challenges. Systematic analysis carried out in this study; improve our understanding of the stability mechanism of asphaltenes. The role of deasphalted crude oil fractions on the stability asphaltene is described.

Keywords: asphaltenes, deasphalting, extraction, vanadium, nickel, metalloporphyrins, ICP-MS, IR spectroscopy

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1200 Synthesis and Characterization of Magnesium and Strontium Doped Sulphate-Hydroxyapatite

Authors: Ammar Z. Alshemary, Yi-Fan Goh, Rafaqat Hussain

Abstract:

Magnesium (Mg2+), strontium (Sr2+) and sulphate ions (SO42-) were successfully substituted into hydroxyapatite (Ca10-x-y MgxSry(PO4)6-z(SO4)zOH2-z) structure through ion exchange process at cationic and anionic sites. Mg2+and Sr2+ ions concentrations were varied between (0.00-0.10), keeping concentration of SO42- ions at z=0.05. [Mg (NO3)2], [Sr (NO3)2] and (Na2SO4) were used as Mg2+, Sr2+, and SO42- sources respectively. The synthesized white precipitate were subjected to heat treatment at 500ºC and finally characterized by X-ray diffraction (XRD) and Fourier Transform infra-red spectroscopy (FTIR). The results showed that the substitution of Mg2+, Sr2+ and SO42- ions into the HA lattice resulted in an increase in the broadness and reduction of XRD peaks. This confirmed that the crystallinity was reduced due to the substitution of ions. Similarly, FTIR result showed the effect of substitution on phosphate bands as well as exchange of hydroxyl group by SO42- ions to balance the charges on HA surface.

Keywords: hydroxyapatite, substitution, characterization, XRD, FTIR

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1199 Synthesis and Characterization of New Polyesters Based on Diarylidene-1-Methyl-4-Piperidone

Authors: Tareg M. Elsunaki, Suleiman A. Arafa, Mohamed A. Abd-Alla

Abstract:

New interesting thermal stable polyesters containing 1-methyl-4-piperidone moiety in the main chain have been synthesized. These polyesters were synthesized by interfacial polycondensation technique of 3,5-bis(4-hydroxybenzylidene)-1-methyl-4-piperidone (I) and 3,5-bis(4-hydroxy-3-methoxy benzyli-dene)-1-methyl-4-piperidone (II) with terphthaloyl, isophthaloyl, 4,4'-diphenic, adipoyl and sebacoyl dichlorides. The yield and the values of the reduced viscosity of the produced polyesters were found to be affected by the type of an organic phase. In order to characterize these polymers, the necessary model compounds (A), (B) were prepared from (I), (II) respectively and benzoyl chloride. The structure of monomers (I), (II), model compounds and resulting polyesters were confirmed by IR, elemental analysis and 1HNMR spectroscopy. The various characteristic of the resulting polymers including solubility, thermal properties, viscosity and X-ray analysis were also studied.

Keywords: synthesis, characterization, new polyesters, chemistry

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1198 Friction Behavior of Wood-Plastic Composites against Uncoated Cemented Carbide

Authors: Almontas Vilutis, Vytenis Jankauskas

Abstract:

The paper presents the results of the investigation of the dry sliding friction of wood-plastic composites (WPCs) against WC-Co cemented carbide. The dependence of the dynamic coefficient of friction on the main influencing factors (vertical load, temperature, and sliding distance) was investigated by evaluating their mutual interaction. Multiple regression analysis showed a high polynomial dependence (adjusted R2 > 0.98). The resistance of the composite to thermo-mechanical effects determines how temperature and force factors affect the magnitude of the coefficient of friction. WPC-B composite has the lowest friction and highest resistance compared to WPC-A, while composite and cemented carbide materials wear the least. Energy dispersive spectroscopy (EDS), based on elemental composition, provided important insights into the friction process.

Keywords: friction, composite, carbide, factors

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1197 Wet Polymeric Precipitation Synthesis for Monophasic Tricalcium Phosphate

Authors: I. Grigoraviciute-Puroniene, K. Tsuru, E. Garskaite, Z. Stankeviciute, A. Beganskiene, K. Ishikawa, A. Kareiva

Abstract:

Tricalcium phosphate (β-Ca3(PO4)2, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.

Keywords: Tricalcium phosphate (β-Ca3(PO4)2, bone regeneration, wet chemical processing, polymeric precipitation

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1196 Eco-Friendly Natural Filler Based Epoxy Composites

Authors: Suheyla Kocaman, Gulnare Ahmetli

Abstract:

In this study, acrylated soybean oil (AESO) was used as modifying agent for DGEBF-type epoxy resin (ER). AESO was used as a co-matrix in 50 wt % with ER. Composites with eco-friendly natural fillers-banana bark and seashell were prepared. MNA was used as a hardener. Effect of banana peel (BP) and seashell (SSh) fillers on mechanical properties, such as tensile strength, elongation at break, and hardness of M-ERs were investigated. The structure epoxy resins (M-ERs) cured with MNA and sebacic acid (SAc) hardeners were characterized by Fourier transform infrared spectroscopy (FTIR). Tensile test results show that Young’s (elastic) modulus, tensile strength and hardness of SSh particles reinforced with M-ERs were higher than the M-ERs reinforced with banana bark.

Keywords: biobased composite, epoxy resin, mechanical properties, natural fillers

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1195 Synthesis of Epoxidized Castor Oil Using a Sulphonated Polystyrene Type Cation Exchange Resin and Its Blend Preparation with Epoxy Resin

Authors: G. S. Sudha, Smita Mohanty, S. K. Nayak

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Epoxidized oils can replace petroleum derived materials in numerous industrial applications, because of their respectable oxirane oxygen content and high reactivity of oxirane ring. Epoxidized castor oil (ECO) has synthesized in the presence of a sulphonated polystyrene type cation exchange resin. The formation of the oxirane ring was confirmed by Fourier Transform Infrared Spectroscopy (FTIR) analysis. The epoxidation reaction was evaluated by Nuclear Magnetic Resonance (NMR) studies. ECO is used as a toughening phase to increase the toughness of petroleum-based epoxy resin.

Keywords: epoxy resin, epoxidized castor oil, sulphonated polystyrene type cation exchange resin, petroleum derived materials

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1194 Speciation of Iron(III) Oxide Nanoparticles and other Paramagnetic Intermediates during High-Temperature Oxidative Pyrolysis of 1-Methylnaphthalene

Authors: M. Paul Herring, Lavrent Khachatryan, Barry Dellinger

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Low Temperature Matrix Isolation - Electron Paramagnetic Resonance (LTMI-EPR) Spectroscopy was utilized to identify the species of iron oxide nanoparticles generated during the oxidative pyrolysis of 1-methylnaphthalene (1-MN). The otherwise gas-phase reactions of 1-MN were impacted by a polypropylenimine tetra-hexacontaamine dendrimer complexed with iron(III) nitrate nonahydrate diluted in air under atmospheric conditions. The EPR fine structure of Fe (III)2O3 nanoparticles clusters, characterized by g-factors of 2.00, 2.28, 3.76 and 4.37 were detected on a cold finger maintained at 77K after accumulation over a multitude of experiments. Additionally, a high valence Fe(IV) paramagnetic intermediate and superoxide anion-radicals, O2•- adsorbed on nanoparticle surfaces in the form of Fe(IV)---O2•- were detected from the quenching area of Zone 1 in the gas-phase.

Keywords: cryogenic trapping, EPFRs, dendrimer, Fe2O3 doped silica, soot

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1193 Evaluation of the Effect Rare Earth Metal on the Microstructure and Properties of Zn-ZnO-Y2O3 Coating of Mild Steel

Authors: A. P. I. Popoola, O. S. I. Fayomi, V. S. Aigbodion

Abstract:

Mild steel has found many engineering applications due to its great formability, availability, low cost and good mechanical properties among others. However its functionality and durability is subject of concern due to corrosion deterioration. Based on these Yttrium is selected as reinforcing particles using electroplating process in this work to enhance the corrosion resistance. Bath formulation of zinc-yttrium was prepared at moderated temperature and pH, to coat mild steel sample. Corrosion and wear behaviour were analyzed using electrochemical potentiostat and abrasive test rig. The composition and microstructure of coated films were investigated standard method. The microstructure of the deposited plate obtained from optimum (10%Yttrium) bath revealed fine-grained deposit of the alloy in the presence of condensation product and hence modified the morphology of zinc–yttrium alloy deposit. It is demonstrated that by adding yttria particles, mild steel can be strengthened with improved polarization behaviour and higher resistance to corrosive in sodium chloride solutions. Microhardness of the coating compared to plain mild steel have increased before and after heat treatment, and an increased wear resistance was also obtained from the modified coating of zinc-yttrium.

Keywords: microhardness, zinc-yttrium, coating, mild steel, microstructure, wear, corrosion

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1192 The Determination of the Zinc Sulfate, Sodium Hydroxide and Boric Acid Molar Ratio on the Production of Zinc Borates

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

Abstract:

Zinc borate is an important boron compound that can be used as multi-functional flame retardant additive due to its high dehydration temperature property. In this study, the raw materials of ZnSO4.7H2O, NaOH and H3BO3 were characterized by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) and used in the synthesis of zinc borates. The synthesis parameters were set to 100°C reaction temperature and 120 minutes of reaction time, with different molar ratio of starting materials (ZnSO4.7H2O:NaOH:H3BO3). After the zinc borate synthesis, the identifications of the products were conducted by XRD and FT-IR. As a result, Zinc Oxide Borate Hydrate [Zn3B6O12.3.5H2O], were synthesized at the molar ratios of 1:1:3, 1:1:4, 1:2:5 and 1:2:6. Among these ratios 1:2:6 had the best results.

Keywords: Zinc borate, ZnSO4.7H2O, NaOH, H3BO3, XRD, FT-IR

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1191 Learning Materials of Atmospheric Pressure Plasma Process: Turning Hydrophilic Surface to Hydrophobic

Authors: C.W. Kan

Abstract:

This paper investigates the use of atmospheric pressure plasma for improving the surface hydrophobicity of polyurethane synthetic leather with tetramethylsilane (TMS). The atmospheric pressure plasma treatment with TMS is a single-step process to enhance the hydrophobicity of polyurethane synthetic leather. The hydrophobicity of the treated surface was examined by contact angle measurement. The physical and chemical surface changes were evaluated by scanning electron microscopy (SEM) and infrared spectroscopy (FTIR). The purpose of this paper is to provide learning materials for understanding how to use atmospheric pressure plasma in the textile finishing process to transform a hydrophilic surface to hydrophobic.

Keywords: Learning materials, atmospheric pressure plasma treatment, hydrophobic, hydrophilic, surface

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1190 Antifungal Activity of Silver Colloidal Nanoparticles against Phytopathogenic Fungus (Phomopsis sp.) in Soybean Seeds

Authors: J. E. Mendes, L. Abrunhosa, J. A. Teixeira, E. R. de Camargo, C. P. de Souza, J. D. C. Pessoa

Abstract:

Among the many promising nanomaterials with antifungal properties, metal nanoparticles (silver nanoparticles) stand out due to their high chemical activity. Therefore, the aim of this study was to evaluate the effect of silver nanoparticles (AgNPs) against Phomopsis sp. AgNPs were synthesized by silver nitrate reduction with sodium citrate and stabilized with ammonia. The synthesized AgNPs have further been characterized by UV/Visible spectroscopy, Biophysical techniques like Dynamic light scattering (DLS) and Scanning Electron Microscopy (SEM). The average diameter of the prepared silver colloidal nanoparticles was about 52 nm. Absolute inhibitions (100%) were observed on treated with a 270 and 540 µg ml-1 concentration of AgNPs. The results from the study of the AgNPs antifungal effect are significant and suggest that the synthesized silver nanoparticles may have an advantage compared with conventional fungicides.

Keywords: antifungal activity, Phomopsis sp., seeds, silver nanoparticles, soybean

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1189 Antibacterial Activity of Nickel Oxide Composite Films with Chitosan/Polyvinyl Chloride/Polyethylene Glycol

Authors: Ali Garba Danjani, Abdulrasheed Halliru Usman

Abstract:

Due to the rapidly increasing biological applications and antibacterial properties of versatile chitosan composites, the effects of chitosan/polyvinyl chloride composites film were investigated. Chitosan/polyvinyl chloride films were prepared by a casting method. Polyethylene glycol (PEG) was used as a plasticizer in the blending stage of film preparation. Characterizations of films were done by Scanning Electron microscopy (SEM), Fourier transforms infrared spectroscopy (FTIR), and thermogravimetric analyzer (TGA). Chitosan composites incorporation enhanced the antibacterial activity of chitosan films against Escherichia coli and Staphylococcus aureus. The composite film produced is proposed as packaging or coating material because of its flexibility, antibacterial efficacy, and good mechanical strength.

Keywords: chitosan, polymeric nanocomposites, antibacterial activity, polymer blend

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1188 Microstructural and Transport Properties of La0.7Sr0.3CoO3 Thin Films Obtained by Metal-Organic Deposition

Authors: K. Daoudi, Z. Othmen, S. El Helali, M.Oueslati, M. Oumezzine

Abstract:

La0.7Sr0.3CoO3 thin films have been epitaxially grown on LaAlO3 and SrTiO3 (001) single-crystal substrates by metal organic deposition process. The structural and micro structural properties of the obtained films have been investigated by means of high resolution X-ray diffraction, Raman spectroscopy and transmission microscopy observations on cross-sections techniques. We noted a close dependence of the crystallinity on the used substrate and the film thickness. By increasing the annealing temperature to 1000ºC and the film thickness to 100 nm, the electrical resistivity was decreased by several orders of magnitude. The film resistivity reaches approximately 3~4 x10-4 Ω.cm in a wide interval of temperature 77-320 K, making this material a promising candidate for a variety of applications.

Keywords: cobaltite, thin films, epitaxial growth, MOD, TEM

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1187 Utilizing Fly Ash Cenosphere and Aerogel for Lightweight Thermal Insulating Cement-Based Composites

Authors: Asad Hanif, Pavithra Parthasarathy, Zongjin Li

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Thermal insulating composites help to reduce the total power consumption in a building by creating a barrier between external and internal environment. Such composites can be used in the roofing tiles or wall panels for exterior surfaces. This study purposes to develop lightweight cement-based composites for thermal insulating applications. Waste materials like silica fume (an industrial by-product) and fly ash cenosphere (FAC) (hollow micro-spherical shells obtained as a waste residue from coal fired power plants) were used as partial replacement of cement and lightweight filler, respectively. Moreover, aerogel, a nano-porous material made of silica, was also used in different dosages for improved thermal insulating behavior, while poly vinyl alcohol (PVA) fibers were added for enhanced toughness. The raw materials including binders and fillers were characterized by X-Ray Diffraction (XRD), X-Ray Fluorescence spectroscopy (XRF), and Brunauer–Emmett–Teller (BET) analysis techniques in which various physical and chemical properties of the raw materials were evaluated like specific surface area, chemical composition (oxide form), and pore size distribution (if any). Ultra-lightweight cementitious composites were developed by varying the amounts of FAC and aerogel with 28-day unit weight ranging from 1551.28 kg/m3 to 1027.85 kg/m3. Excellent mechanical and thermal insulating properties of the resulting composites were obtained ranging from 53.62 MPa to 8.66 MPa compressive strength, 9.77 MPa to 3.98 MPa flexural strength, and 0.3025 W/m-K to 0.2009 W/m-K as thermal conductivity coefficient (QTM-500). The composites were also tested for peak temperature difference between outer and inner surfaces when subjected to heating (in a specially designed experimental set-up) by a 275W infrared lamp. The temperature difference up to 16.78 oC was achieved, which indicated outstanding properties of the developed composites to act as a thermal barrier for building envelopes. Microstructural studies were carried out by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) for characterizing the inner structure of the composite specimen. Also, the hydration products were quantified using the surface area mapping and line scale technique in EDS. The microstructural analyses indicated excellent bonding of FAC and aerogel in the cementitious system. Also, selective reactivity of FAC was ascertained from the SEM imagery where the partially consumed FAC shells were observed. All in all, the lightweight fillers, FAC, and aerogel helped to produce the lightweight composites due to their physical characteristics, while exceptional mechanical properties, owing to FAC partial reactivity, were achieved.

Keywords: aerogel, cement-based, composite, fly ash cenosphere, lightweight, sustainable development, thermal conductivity

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1186 E-Tongue Based on Metallo-Porphyrins for Histamine Evaluation

Authors: A. M. Iordache, S. M. Iordache, V. Barna, M. Elisa, I. C. Vasiliu, C. R. Stefan, I. Chilibon, I. Stamatin, S. Caramizoiu, C. E. A. Grigorescu

Abstract:

The general objective of the presentation is the development of an e-tongue like sensor based on modified screen printed electrode (SPE) structures with a receptor part made of porphyrins/metalloporphyrins chemically bound to graphene (the sensitive assembly) to act as antennas and “capture” the histamine molecules. Using a single, ultra-sensitive electrochemical sensor, we measured the concentration of histamine, a compound which is strongly connected to the level of freshness in foods (the caution level of histamine is 50 ppm, whereas the maximum accepted levels range from 200 ppm to 500 ppm). Our approach for the chemical immobilization of the porphyrins onto the surface of the graphenes was via substitution reaction: a solution of graphene in SOCl2 was heated to 800C for 6 hours. Upon cooling, the metallo-porphyrins were added and ultrasonicated for 4 hours. The solution was then allowed to cool to room temperature and then centrifuged in order to separate the deposit. The sensitive assembly was drop casted onto the carbon SPE and cyclic voltammetry was performed in the presence of histamine. The reaction is quasi-reversible and the sensor showed an oxidation potential for histamine at 600 mV. The results indicate a linear dependence of concentration of histamine as function of intensity. The results are reproducible; however the chemical stability of the sensitive assembly is low.

Keywords: histamine, cyclic voltammetry, metallo-porphyrin, food freshness

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1185 Chemical Bath Deposition Technique (CBD) of Cds Used in Closed Space Sublimation (CSS) of CdTe Solar Cell

Authors: Zafar Mahmood, Fahimullah Babar, Surriyia Naz, Hafiz Ur Rehman

Abstract:

Cadmium Sulphide (CdS) was deposited on a Tec 15 glass substrate with the help of CBD (chemical bath deposition process) and then cadmium telluride CdTe was deposited on CdS with the help of CSS (closed spaced sublimation technique) for the construction of a solar cell. The thicknesses of all the deposited materials were measured with the help of Elipsometry. The IV graphs were drawn in order to observe the current voltage output. The efficiency of the cell was graphed with the fill factor as well (graphs not given here).The efficiency came out to be approximately 16.5 % and the CIGS (copper- indium –gallium- selenide) maximum efficiency is 20 %.The efficiency of a solar cell can further be enhanced by adapting quality materials, good experimental devices and proper procedures. The grain size was analyzed with the help of scanning electron microscope using RBS (Rutherford backscattering spectroscopy).

Keywords: CBD, CdS, CdTe, CSS

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1184 Free Fatty Acid Assessment of Crude Palm Oil Using a Non-Destructive Approach

Authors: Siti Nurhidayah Naqiah Abdull Rani, Herlina Abdul Rahim, Rashidah Ghazali, Noramli Abdul Razak

Abstract:

Near infrared (NIR) spectroscopy has always been of great interest in the food and agriculture industries. The development of prediction models has facilitated the estimation process in recent years. In this study, 110 crude palm oil (CPO) samples were used to build a free fatty acid (FFA) prediction model. 60% of the collected data were used for training purposes and the remaining 40% used for testing. The visible peaks on the NIR spectrum were at 1725 nm and 1760 nm, indicating the existence of the first overtone of C-H bands. Principal component regression (PCR) was applied to the data in order to build this mathematical prediction model. The optimal number of principal components was 10. The results showed R2=0.7147 for the training set and R2=0.6404 for the testing set.

Keywords: palm oil, fatty acid, NIRS, regression

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1183 Modified DNA as a Base Material for Nonlinear Optics

Authors: Ewelina Nowak, Anna Wisla-Swider

Abstract:

Deoxyribonucleic acid (DNA) is a biomolecule which exhibits an electro-optic properties. These features are related with structure of double-stranded helix. Modification of DNA with ionic liquids allows intensify these properties. The aim of our study was synthesis of ionic liquids that are used the formation of DNA-surfactant complexes in order to obtain new materials with potential application for nonlinear optics. Complexes were achieved through the ion exchange reactions of carbazole-based and imidazole-based ionic liquids with H+ ions from salmon DNA. To examination the properties of obtained complexes DNA-ionic liquids there were investigated using circular dichroism (CD), UV-Vis spectra and infrared spectroscopy (IR). Additionally, the resulting DNA-surfactant complexes were characterized in terms of solubility in common organic solvents and water.

Keywords: deoxyribonucleic acid, biomolecule, carbazole, imidazole, ionic liquids, ion exchange reactions

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1182 Development of Sulfite Biosensor Based on Sulfite Oxidase Immobilized on 3-Aminoproplytriethoxysilane Modified Indium Tin Oxide Electrode

Authors: Pawasuth Saengdee, Chamras Promptmas, Ting Zeng, Silke Leimkühler, Ulla Wollenberger

Abstract:

Sulfite has been used as a versatile preservative to limit the microbial growth and to control the taste in some food and beverage. However, it has been reported to cause a wide spectrum of severe adverse reactions. Therefore, it is important to determine the amount of sulfite in food and beverage to ensure consumer safety. An efficient electrocatalytic biosensor for sulfite detection was developed by immobilizing of human sulfite oxidase (hSO) on 3-aminoproplytriethoxysilane (APTES) modified indium tin oxide (ITO) electrode. Cyclic voltammetry was employed to investigate the electrochemical characteristics of the hSO modified ITO electrode for various pretreatment and binding conditions. Amperometry was also utilized to demonstrate the current responses of the sulfite sensor toward sodium sulfite in an aqueous solution at a potential of 0 V (vs. Ag/AgCl 1 M KCl). The proposed sulfite sensor has a linear range between 0.5 to 2 mM with a correlation coefficient 0.972. Then, the additional polymer layer of PVA was introduced to extend the linear range of sulfite sensor and protect the enzyme. The linear range of sulfite sensor with 5% coverage increases from 2.8 to 20 mM at a correlation coefficient of 0.983. In addition, the stability of sulfite sensor with 5% PVA coverage increases until 14 days when kept in 0.5 mM Tris-buffer, pH 7.0 at 4 8C. Therefore, this sensor could be applied for the detection of sulfite in the real sample, especially in food and beverage.

Keywords: sulfite oxidase, bioelectrocatalytsis, indium tin oxide, direct electrochemistry, sulfite sensor

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1181 Graphene-Oxide-Supported Coal-Layered Double Hydroxides: Synthesis and Characterizations

Authors: Shaeel A. Al Thabaiti, Sulaiman N. Basahel, Salem M. Bawaked, Mohamed Mokhtar

Abstract:

Nanosheets for cobalt-layered double hydroxide (Co-Al-LDH)/GO were successfully synthesized with different Co:M g:Al ratios (0:3:1, 1.5:1.5:1, and 3:0:1). The layered double hydroxide structure and morphology were determined using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Temperature prgrammed reduction (TPR) of Co-Al-LDH showed reduction peaks at lower temperature which indicates the ease reducibility of this particular sample. The thermal behaviour was studied using thermal graviemetric technique (TG), and the BET-surface area was determined using N2 physisorption at -196°C. The C-C coupling reaction was carried out over all the investigated catalysts. The Mg–Al LDH catalyst without Co ions is inactive, but the isomorphic substitution of Mg by Co ions (Co:Mg:Al = 1.5:1.5:1) in the cationic sheet resulted in 88% conversion of iodobenzene under reflux. LDH/GO hybrid is up to 2 times higher activity than for the unsupported LDH.

Keywords: adsorption, co-precipitation, graphene oxide, layer double hydroxide

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1180 Heavy Metals in PM2.5 Aerosols in Urban Sites of Győr, Hungary

Authors: Zs. Csanádi, A. Szabó Nagy, J. Szabó, J. Erdős

Abstract:

Atmospheric concentrations of some heavy metal compounds (Pb, Cd, Ni) and the metalloid As were identified and determined in airborne PM2.5 particles in urban sites of Győr, northwest area of Hungary. PM2.5 aerosol samples were collected in two different sampling sites and the trace metal(loid) (Pb, Ni, Cd and As) content were analyzed by atomic absorption spectroscopy. The concentration of PM2.5 fraction was varied between 12.22 and 36.92 μg/m3 at the two sampling sites. The trend of heavy metal mean concentrations regarding the mean value of the two urban sites of Győr was found in decreasing order of Pb > Ni > Cd. The mean values were 7.59 ng/m3 for Pb, 0.34 ng/m3 for Ni and 0.11 ng/m3 for Cd, respectively. The metalloid As could be detected only in 3.57% of the total collected samples. The levels of PM2.5 bounded heavy metals were determined and compared with other cities located in Hungary.

Keywords: aerosol, air quality, heavy metals, PM2.5

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1179 The Optimization of Copper Sulfate and Tincalconite Molar Ratios on the Hydrothermal Synthesis of Copper Borates

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

Abstract:

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

Keywords: hydrothermal synthesis, copper borates, copper sulfate, tincalconite

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1178 Structural, Optical and Electrical Properties of PbS Thin Films Deposited by CBD at Different Bath pH

Authors: Lynda Beddek, Nadhir Attaf, Mohamed Salah Aida

Abstract:

PbS thin films were grown on glass substrates by chemical bath deposition (CBD). The precursor aqueous bath contained 1 mole of lead nitrate, 1 mole of Thiourea and complexing agents (triethanolamine (TEA) and NaOH). Bath temperature and deposition time were fixed at 60°C and 3 hours, respectively. However, the PH of bath was varied from 10.5 to 12.5. Structural properties of the deposited films were characterized by X-ray diffraction and Raman spectroscopy. The preferred direction was revealed to be along (111) and the PbS crystal structure was confirmed. Strains and grains sizes were also calculated. Optical studies showed that films thicknesses do not exceed 600nm. Energy band gap values of films decreases with increase in pH and reached a value ~ 0.4eV at pH equal 12.5. The small value of the energy band gap makes PbS one of the most interesting candidate for solar energy conversion near the infrared ray.

Keywords: CBD, PbS, pH, thin films, x-ray diffraction

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1177 Measurement of 238U, 232Th and 40K in Soil Samples Collected from Coal City Dhanbad, India

Authors: Zubair Ahmad

Abstract:

Specific activities of the natural radionuclides 238U, 232Th and 40K were measured by using γ - ray spectrometric technique in soil samples collected from the city of Dhanbad, which is located near coal mines. Mean activity values for 238U, 232Th and 40K were found to be 60.29 Bq/kg, 64.50 Bq/kg and 481.0 Bq/kg, respectively. Mean radium equivalent activity, absorbed dose rate, outdoor dose, external hazard index, internal hazard index, for the area under study were determined as 189.53 Bq/kg, 87.21 nGy/h, 0.37 mSv/y, 0.52 and 0.64, respectively. The annual effective dose to the general public was found 0.44 mSv/y. This value lies well below the limit of 1 mSv/y as recommended by International Commission on Radiological Protection. Measured values were found safe for environment and public health.

Keywords: coal city Dhanbad, gamma-ray spectroscopy, natural radioactivity, soil samples

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1176 The Mechanical and Electrochemical Properties of DC-Electrodeposited Ni-Mn Alloy Coating with Low Internal Stress

Authors: Chun-Ying Lee, Kuan-Hui Cheng, Mei-Wen Wu

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The nickel-manganese (Ni-Mn) alloy coating prepared from DC electrodeposition process in sulphamate bath was studied. The effects of process parameters, such as current density and electrolyte composition, on the cathodic current efficiency, microstructure, internal stress and mechanical properties were investigated. Because of its crucial effect on the application to the electroforming of microelectronic components, the development of low internal stress coating with high leveling power was emphasized. It was found that both the coating’s manganese content and the cathodic current efficiency increased with the raise in current density. In addition, the internal stress of the deposited coating showed compressive nature at low current densities while changed to tensile one at higher current densities. Moreover, the metallographic observation, X-ray diffraction measurement, transmission electron microscope (TEM) examination, and polarization curve measurement were conducted. It was found that the Ni-Mn coating consisted of nano-sized columnar grains and the maximum hardness of the coating was associated with (111) preferred orientation in the microstructure. The grain size was refined along with the increase in the manganese content of the coating, which accordingly, raised its hardness and mechanical tensile strength. In summary, the Ni-Mn coating prepared at lower current density of 1-2 A/dm2 had low internal stress, high leveling power, and better corrosion resistance.

Keywords: Ni-Mn coating, DC plating, internal stress, leveling power

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1175 Nitrate Photoremoval in Water Using Nanocatalysts Based on Ag / Pt over TiO2

Authors: Ana M. Antolín, Sandra Contreras, Francesc Medina, Didier Tichit

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Introduction: High levels of nitrates (> 50 ppm NO3-) in drinking water are potentially risky to human health. In the recent years, the trend of nitrate concentration in groundwater is rising in the EU and other countries. Conventional catalytic nitrate reduction processes into N2 and H2O lead to some toxic intermediates and by-products, such as NO2-, NH4+, and NOx gases. Alternatively, photocatalytic nitrate removal using solar irradiation and heterogeneous catalysts is a very promising and ecofriendly technique. It has been scarcely performed and more research on highly efficient catalysts is still needed. In this work, different nanocatalysts supported on Aeroxide Titania P25 (P25) have been prepared varying: 0.5-4 % wt. Ag); Pt (2, 4 % wt.); Pt precursor (H2PtCl6/K2PtCl6); and impregnation order of both metals. Pt was chosen in order to increase the selectivity to N2 and decrease that to NO2-. Catalysts were characterized by nitrogen physisorption, X-Ray diffraction, UV-visible spectroscopy, TEM and X Ray-Photoelectron Spectroscopy. The aim was to determine the influence of the composition and the preparation method of the catalysts on the conversion and selectivity in the nitrate reduction, as well as going through an overall and better understanding of the process. Nanocatalysts synthesis: For the mono and bimetallic catalysts preparation, wise-drop wetness impregnation of the precursors (AgNO3, H2PtCl6, K2PtCl6) followed by a reduction step (NaBH4) was used to obtain the metal colloids. Results and conclusions: Denitration experiments were performed in a 350 mL PTFE batch reactor under inert standard operational conditions, ultraviolet irradiations (λ=254 nm (UV-C); λ=365 nm (UV-A)), and presence/absence of hydrogen gas as a reducing agent, contrary to most studies using oxalic or formic acid. Samples were analyzed by Ionic Chromatography. Blank experiments using respectively P25 (dark conditions), hydrogen only and UV irradiations without hydrogen demonstrated a clear influence of the presence of hydrogen on nitrate reduction. Also, they demonstrated that UV irradiation increased the selectivity to N2. Interestingly, the best activity was obtained under ultraviolet lamps, especially at a closer wavelength to visible light irradiation (λ = 365 nm) and H2. 2% Ag/P25 leaded to the highest NO3- conversion among the monometallic catalysts. However, nitrite quantities have to be diminished. On the other hand, practically no nitrate conversion was observed with the monometallics based on Pt/P25. Therefore, the amount of 2% Ag was chosen for the bimetallic catalysts. Regarding the bimetallic catalysts, it is observed that the metal impregnation order, amount and Pt precursor highly affects the results. Higher selectivity to the desirable N2 gas is obtained when Pt was firstly added, especially with K2PtCl6 as Pt precursor. This suggests that when Pt is secondly added, it covers the Ag particles, which are the most active in this reaction. It could be concluded that Ag allows the nitrate reduction step to nitrite, and Pt the nitrite reduction step toward the desirable N2 gas.

Keywords: heterogeneous catalysis, hydrogenation, nanocatalyst, nitrate removal, photocatalysis

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1174 Effect of Nitriding and Shot Peening on Corrosion Behavior and Surface Properties of Austenite Stainless Steel 316L

Authors: Khiaira S. Hassan, Abbas S. Alwan, Muna K. Abbass

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This research aims to study the effect of the liquid nitriding and shot peening on the hardness, surface roughness, residual stress, microstructure and corrosion behavior of austenite stainless steel 316 L. Chemical surface heat treatment by liquid nitriding process was carried out at 500 °C for 1 h and followed by shot peening with using ball steel diameter of 1.25 mm in different exposure time of 10 and 20 min. Electrochemical corrosion test was applied in sea water (3.5% NaCl solution) by using potentostat instrument. The results showed that the nitride layer consists of a compound layer (white layer) and diffusion zone immediately below the alloy layer. It has been found that the mechanical treatment (shot peening) has led to the formation of compressive residual stresses in layer surface that increased the hardness of stainless steel surface. All surface treatment (nitriding and shot peening) processes have led to the formation of carbide of CrN in hard surface layer. It was shown that both processes caused an increase in surface hardness and roughness which increases with shot peening time. Also, the corrosion results showed that the liquid nitriding and shot peening processes increase the corrosion rate to values more than that of not treated stainless steel.

Keywords: stainless steel 316L, shot peening, nitriding, corrosion, hardness

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1173 Ultrasensitive Hepatitis B Virus Detection in Blood Using Nano-Porous Silicon Oxide: Towards POC Diagnostics

Authors: N. Das, N. Samanta, L. Pandey, C. Roy Chaudhuri

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Early diagnosis of infection like Hep-B virus in blood is important for low cost medical treatment. For this purpose, it is desirable to develop a point of care device which should be able to detect trace quantities of the target molecule in blood. In this paper, we report a nanoporous silicon oxide sensor which is capable of detecting down to 1fM concentration of Hep-B surface antigen in blood without the requirement of any centrifuge or pre-concentration. This has been made possible by the presence of resonant peak in the sensitivity characteristics. This peak is observed to be dependent only on the concentration of the specific antigen and not on the interfering species in blood serum. The occurrence of opposite impedance change within the pores and at the bottom of the pore is responsible for this effect. An electronic interface has also been designed to provide a display of the virus concentration.

Keywords: impedance spectroscopy, ultrasensitive detection in blood, peak frequency, electronic interface

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1172 Phytochemical and Antimicrobial Properties of Zinc Oxide Nanocomposites on Multidrug-Resistant E. coli Enzyme: In-vitro and in-silico Studies

Authors: Callistus I. Iheme, Kenneth E. Asika, Emmanuel I. Ugwor, Chukwuka U. Ogbonna, Ugonna H. Uzoka, Nneamaka A. Chiegboka, Chinwe S. Alisi, Obinna S. Nwabueze, Amanda U. Ezirim, Judeanthony N. Ogbulie

Abstract:

Antimicrobial resistance (AMR) is a major threat to the global health sector. Zinc oxide nanocomposites (ZnONCs), composed of zinc oxide nanoparticles and phytochemicals from Azadirachta indica aqueous leaf extract, were assessed for their physico-chemicals, in silico and in vitro antimicrobial properties on multidrug-resistant Escherichia coli enzymes. Gas chromatography coupled with mass spectroscope (GC-MS) analysis on the ZnONCs revealed the presence of twenty volatile phytochemical compounds, among which is scoparone. Characterization of the ZnONCs was done using ultraviolet-visible spectroscopy (UV-vis), energy dispersive spectroscopy (EDX), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and x-ray diffractometer (XRD). Dehydrogenase enzyme converts colorless 2,3,5-triphenyltetrazolium chloride to the red triphenyl formazan (TPF). The rate of formazan formation in the presence of ZnONCs is proportional to the enzyme activities. The color formation is extracted and determined at 500 nm, and the percentage of enzyme activity is calculated. To determine the bioactive components of the ZnONCs, characterize their binding to enzymes, and evaluate the enzyme-ligand complex stability, respectively Discrete Fourier Transform (DFT) analysis, docking, and molecular dynamics simulations will be employed. The results showed arrays of ZnONCs nanorods with maximal absorption wavelengths of 320 nm and 350 nm and thermally stable at the temperature range of 423.77 to 889.69 ℃. In vitro study assessed the dehydrogenase inhibitory properties of the ZnONCs, conjugate of ZnONCs and ampicillin (ZnONCs-amp), the aqueous leaf extract of A. indica, and ampicillin (standard drug). The findings revealed that at the concentration of 500 μm/mL, 57.89 % of the enzyme activities were inhibited by ZnONCs compared to 33.33% and 21.05% of the standard drug (Ampicillin), and the aqueous leaf extract of the A. indica respectively. The inhibition of the enzyme activities by the ZnONCs at 500 μm/mL was further enhanced to 89.74 % by conjugating with Ampicillin. In silico study on the ZnONCs revealed scoparone as the most viable competitor of nicotinamide adenine dinucleotide (NAD⁺) for the coenzyme binding pocket on E. coli malate and histidinol dehydrogenase. From the findings, it can be concluded that the scoparone components of the nanocomposites in synergy with the zinc oxide nanoparticles inhibited E. coli malate and histidinol dehydrogenase by competitively binding to the NAD⁺ pocket and that the conjugation of the ZnONCs with ampicillin further enhanced the antimicrobial efficiency of the nanocomposite against multidrug resistant E. coli.

Keywords: antimicrobial resistance, dehydrogenase activities, E. coli, zinc oxide nanocomposites

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