Search results for: Impedance Spectroscopy

Authors: Oluwole Opeyemi Dina, Saheed E. Elugoke, Peter Olutope Fayemi, Omolola E. Fayemi

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This study presents the detection of epinephrine (EP) at Fe₃O₄ modified screen printed silver electrode (SPSE). The iron oxide (Fe₃O₄) nanoparticles were characterized with UV-visible spectroscopy, Fourier-Transform infrared spectroscopy (FT-IR) and Scanning electron microscopy (SEM) prior to the modification of the SPSE. The EP oxidation peak current (Iap) increased with an increase in the concentration of EP as well as the scan rate (from 25 - 400 mVs⁻¹). Using cyclic voltammetry (CV), the relationship between Iap and EP concentration was linear over a range of 3.8 -118.9 µM and 118.9-175 µM with a detection limit of 41.99 µM and 83.16 µM, respectively. Selective detection of EP in the presence of ascorbic acid was also achieved at this electrode.

Keywords: screenprint electrode, iron oxide nanoparticle, epinephrine, serum, cyclic voltametry

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Authors: Dina Ahmed Selim, Eman Shawky Anwar, Rasha Mohamed Abu El-Khair

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A rapid, simple and efficient method with minimal sample treatment was developed for authentication of Garcinia cambogia fruit peel powder, along with determining undeclared active pharmaceutical ingredients (APIs) in its herbal slimming dietary supplements using near infrared spectroscopy combined with chemometrics. Five featured adulterants, including sibutramine, metformin, orlistat, ephedrine, and theophylline are selected as target compounds. The Near infrared spectral data matrix of authentic Garcinia cambogia fruit peel and specimens degraded by intentional contamination with the five selected APIs was subjected to hierarchical clustering analysis to investigate their bundling figure. SIMCA models were established to ensure the genuiness of Garcinia cambogia fruit peel which resulted in perfect classification of all tested specimens. Adulterated samples were utilized for construction of PLSR models based on different APIs contents at minute levels of fraud practices (LOQ < 0.2% w/w).The suggested approach can be applied to enhance and guarantee the safety and quality of Garcinia fruit peel powder as raw material and in dietary supplements.

Keywords: Garcinia cambogia, Quality control, NIR spectroscopy, Chemometrics

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Authors: Mourad Makhlouf, Bouabdellah Benaicha, Zoubir Benmaamar, Didier Villemin

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The addition of combustion catalysts to ammonium perchlorate-based composite fuels can indeed significantly enhance their performance. In this work, a nanocomposite was synthesized using graphene oxide (GO) and hematite nanoparticles grafted onto graphene oxide as a catalyst support.To characterize the nanocomposite, several experimental techniques were employed, including Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM). FTIR is useful for analyzing chemical bonding and functional groups, while Raman spectroscopy provides information about the vibrational modes of the materials. SEM allows for visualizing the surface morphology and structure.The thermal analysis of two mixtures, one based on AP/GO and the other on AP/GO-Fe2O3, was conducted with varying percentages. The results indicated that the nanocomposite GO-Fe2O3 acted as a catalyst, significantly accelerating the thermal decomposition process of AP. This catalytic effect ultimately led to an improvement in the energy performance of the composite fuel.Overall, the synthesis and characterization of the nanocomposite, as well as the thermal analysis, demonstrated the effectiveness of GO-Fe2O3 as a combustion catalyst in enhancing the performance of ammonium perchlorate-based composite fuels.

Keywords: composite propellants, ammonium perchlorate, nanocomposite, catalytic support, hematite nanoparticles, graphene oxide, thermal decomposition

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Authors: Peter Kus, Anna Ostroverkh, Yurii Yakovlev, Yevheniia Lobko, Roman Fiala, Ivan Khalakhan, Vladimir Matolin

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Hydrogen economy is a concept of low-emission society which harvests most of its energy from renewable sources (e.g., wind and solar) and in case of overproduction, electrochemically turns the excess amount into hydrogen, which serves as an energy carrier. Proton exchange membrane water electrolyzers (PEMWE) are the backbone of this concept. By fast-response electricity to hydrogen conversion, the PEMWEs will not only stabilize the electrical grid but also provide high-purity hydrogen for variety of fuel cell powered devices, ranging from consumer electronics to vehicles. Wider commercialization of PEMWE technology is however hindered by high prices of noble metals which are necessary for catalyzing the redox reactions within the cell. Namely, platinum for hydrogen evolution reaction (HER), running on cathode, and iridium for oxygen evolution reaction (OER) on anode. Possible way of how to lower the loading of Pt and Ir is by using conductive high-surface nanostructures as catalyst supports in conjunction with thin-film catalyst deposition. The presented study discusses unconventional technique of membrane electron assembly (MEA) preparation. Noble metal catalysts (Pt and Ir) were magnetron sputtered in very low loadings onto the surface of porous sublayers (located on gas diffusion layer or directly on membrane), forming so to say localized three-phase boundary. Ultrasonically sprayed corrosion resistant TiC-based sublayer was used as a support material on anode, whereas magnetron sputtered nanostructured etched nitrogenated carbon (CNx) served the same role on cathode. By using this configuration, we were able to significantly decrease the amount of noble metals (to thickness of just tens of nanometers), while keeping the performance comparable to that of average state-of-the-art catalysts. Complex characterization of prepared supported catalysts includes in-cell performance and durability tests, electrochemical impedance spectroscopy (EIS) as well as scanning electron microscopy (SEM) imaging and X-ray photoelectron spectroscopy (XPS) analysis. Our research proves that magnetron sputtering is a suitable method for thin-film deposition of electrocatalysts. Tested set-up of thin-film supported anode and cathode catalysts with combined loading of just 120 ug.cm⁻² yields remarkable values of specific current. Described approach of thin-film low-loading catalyst deposition might be relevant when noble metal reduction is the topmost priority.

Keywords: hydrogen economy, low-loading catalyst, magnetron sputtering, proton exchange membrane water electrolyzer

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Authors: Shari Ann S. Botin, Ruziel Larmae T. Gimpaya, Rembrant Rockwell Gamboa, Rinlee Butch M. Cervera

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In recent years, demand for the use of solid electrolytes as alternatives to liquid electrolytes has increased due to recurring battery safety and stability issues, in addition to an increase in energy density requirement which can be made possible by using solid electrolytes. Among the solid electrolyte systems, Li7La3Zr2O12 (LLZ) is one of the most promising as it exhibits good chemical stability against Li metal and has a relatively high ionic conductivity. In this study, pure and doped LLZ were synthesized via conventional solid state reaction. The precursor chemicals (such as LiOH, La2O3, Ga2O3 and ZrO2) were ground and then calcined at 900 °C, pressed into pellets and finally sintered at 1000 °C to 1200 °C. The microstructure and ionic conductivity of the obtained samples have been investigated. Results show that for pure LLZ, sintering at lower temperature (1000 °C) produced tetragonal LLZ while sintering at higher temperatures (≥ 1150 °C) produced cubic LLZ based from the XRD results. However, doping with Ga produces an easier formation of LLZ with cubic structure at lower sintering duration. On the other hand, the lithium conductivity of the samples was investigated using electrochemical impedance spectroscopy at room temperature. Among the obtained samples, Ga-doped LLZ sintered at 1150 °C obtained the highest ionic conductivity reaching to about 1x10⁻⁴ S/cm at room temperature. In addition, fabrication and initial investigation of an all-solid state Lithium Battery using the synthesized LLZ sample with the use of commercial cathode materials have been investigated.

Keywords: doped LLZ, lithium-ion battery, pure LLZ, solid electrolytes

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Authors: Dana Alina Magdas, Nicoleta Simona Vedeanu, Ioana Feher, Rares Stiufiuc

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Food and beverages authentication using rapid and non-expensive analytical tools represents nowadays an important challenge. In this regard, the potential of vibrational techniques in food authentication has gained an increased attention during the last years. For wines discrimination, Raman spectroscopy appears more feasible to be used as compared with IR (infrared) spectroscopy, because of the relatively weak water bending mode in the vibrational spectroscopy fingerprint range. Despite this, the use of Raman technique in wine discrimination is in an early stage. Taking this into consideration, the wine discrimination potential of surface-enhanced Raman scattering (SERS) technique is reported in the present work. The novelty of this study, compared with the previously reported studies, concerning the application of vibrational techniques in wine discrimination consists in the fact that the present work presents the wines differentiation based on the individual signals obtained from deconvoluted spectra. In order to achieve wines classification with respect to variety, geographical origin and vintage, the peaks intensities obtained after spectra deconvolution were compared using supervised chemometric methods like Linear Discriminant Analysis (LDA). For this purpose, a set of 20 white Romanian wines from different viticultural Romanian regions four varieties, was considered. Chemometric methods applied directly to row SERS experimental spectra proved their efficiency, but discrimination markers identification found to be very difficult due to the overlapped signals as well as for the band shifts. By using this approach, a better general view related to the differences that appear among the wines in terms of compositional differentiation could be reached.

Keywords: chemometry, SERS, variety, wines discrimination

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Authors: Takoua Soltani, Imen Soltani, Taoufik Aguili

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The communications' and radar systems' demands give rise to new developments in the domain of active integrated antennas (AIA) and arrays. The main advantages of AIA arrays are the simplicity of fabrication, low cost of manufacturing, and the combination between free space power and the scanner without a phase shifter. The integrated active antenna modeling is the coupling between the electromagnetic model and the transport model that will be affected in the high frequencies. Global modeling of active circuits is important for simulating EM coupling, interaction between active devices and the EM waves, and the effects of EM radiation on active and passive components. The current review focuses on the modeling of the active element which is a MESFET transistor immersed in a rectangular waveguide. The proposed EM analysis is based on the Method of Moments combined with the Generalised Equivalent Circuit method (MOM-GEC). The Method of Moments which is the most common and powerful software as numerical techniques have been used in resolving the electromagnetic problems. In the class of numerical techniques, MOM is the dominant technique in solving of Maxwell and Transport’s integral equations for an active integrated antenna. In this situation, the equivalent circuit is introduced to the development of an integral method formulation based on the transposition of field problems in a Generalised equivalent circuit that is simpler to treat. The method of Generalised Equivalent Circuit (MGEC) was suggested in order to represent integral equations circuits that describe the unknown electromagnetic boundary conditions. The equivalent circuit presents a true electric image of the studied structures for describing the discontinuity and its environment. The aim of our developed method is to investigate the antenna parameters such as the input impedance and the current density distribution and the electric field distribution. In this work, we propose a global EM modeling of the MESFET AsGa transistor using an integral method. We will begin by describing the modeling structure that allows defining an equivalent EM scheme translating the electromagnetic equations considered. Secondly, the projection of these equations on common-type test functions leads to a linear matrix equation where the unknown variable represents the amplitudes of the current density. Solving this equation resulted in providing the input impedance, the distribution of the current density and the electric field distribution. From electromagnetic calculations, we were able to present the convergence of input impedance for different test function number as a function of the guide mode numbers. This paper presents a pilot study to find the answer to map out the variation of the existing current evaluated by the MOM-GEC. The essential improvement of our method is reducing computing time and memory requirements in order to provide a sufficient global model of the MESFET transistor.

Keywords: active integrated antenna, current density, input impedance, MESFET transistor, MOM-GEC method

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Authors: B. Kurbanova, M. Karibayev, N. Almas, K. Ospanov, K. Aimaganbetov, T. Kuanyshbekov, K. Akatan, S. Kabdrakhmanova

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Proton exchange membranes (PEMs) operating at high temperatures above 100 °C with the excellent mechanical, chemical and thermochemical stability have been received much attention, because of their practical application of proton exchange membrane fuel cells (PEMFCs). Nowadays, a huge number of polymers and polymer-mixed various membranes have been investigated for this application, all of which offer both pros and cons. However, PEMFCs are still lack of ideal membranes with unique properties. In this work, carboxymethylcellulose (CMC) based membranes with dispersive graphene oxide (GO) sheets were fabricated and investigated for PEMFCs application. These membranes and pristine GO were studied by a combination of XRD, XPS, Raman, Brillouin, FTIR, thermo-mechanical analysis (TGA and Dynamic Mechanical Analysis) and SEM microscopy, while substantial studies on the proton transport properties were provided by Electrochemical Impedance Spectroscopy (EIS) measurements. It was revealed that the addition of CMC to the GO boosts proton conductivity of the whole membrane, while GO provides good mechanical and thermomechanical stability to the membrane. Further, the continuous and ordered nanochannels with well-tailored chemical structures were obtained by irradiation of heavy ions Kr⁺¹⁷ with an energy of 1.75 MeV/nucleon on the heavy ion accelerator. The formation of these nanochannels led to the significant increase of proton conductivity at 50% Relative Humidity. Also, FTIR and XPS measurement results show that ion irradiation eliminated the GO’s surface oxygen chemical bonds (C=O, C-O), and led to the formation of C = C, C – C bonds, whereas these changes connected with an increase in conductivity.

Keywords: proton exchange membranes, graphene oxide, fuel cells, carboxymethylcellulose, ion irradiation

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Authors: Akhtar Rasool, Tasneem Zahra Rizvi

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In this study, a series of the cadmium sulphide quantum dots/polyaniline nanocomposites with varying compositions were prepared by in-situ polymerization technique and were characterized using X-ray diffraction and Fourier transform infrared spectroscopy. The surface morphology was studied by scanning electron microscopy. UV-Visible spectroscopy was used to find out the energy band gap of the nanoparticles and the nanocomposites. Temperature dependence of DC electrical conductivity and temperature and frequency dependence of AC conductivity were investigated to study the charge transport mechanism in the nanocomposites. DC conductivity was found to be a typical for a semiconducting behavior following Mott’s 1D variable range hoping model. The frequency dependent AC conductivity followed the universal power law.

Keywords: conducting polymers, nanocomposites, polyaniline composites, quantum dots

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Authors: Amanda T. Badaró, Douglas F. Barbin, Sofia T. Garcia, Maria Teresa P. S. Clerici, Amanda R. Ferreira

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Food fortification is the intentional addition of a nutrient in a food matrix and has been widely used to overcome the lack of nutrients in the diet or increasing the nutritional value of food. Fortified food must meet the demand of the population, taking into account their habits and risks that these foods may cause. Wheat and its by-products, such as semolina, has been strongly indicated to be used as a food vehicle since it is widely consumed and used in the production of other foods. These products have been strategically used to add some nutrients, such as fibers. Methods of analysis and quantification of these kinds of components are destructive and require lengthy sample preparation and analysis. Therefore, the industry has searched for faster and less invasive methods, such as Near-Infrared Spectroscopy (NIR). NIR is a rapid and cost-effective method, however, it is based on indirect measurements, yielding high amount of data. Therefore, NIR spectroscopy requires calibration with mathematical and statistical tools (Chemometrics) to extract analytical information from the corresponding spectra, as Principal Component Analysis (PCA) and Linear Discriminant Analysis (LDA). PCA is well suited for NIR, once it can handle many spectra at a time and be used for non-supervised classification. Advantages of the PCA, which is also a data reduction technique, is that it reduces the data spectra to a smaller number of latent variables for further interpretation. On the other hand, LDA is a supervised method that searches the Canonical Variables (CV) with the maximum separation among different categories. In LDA, the first CV is the direction of maximum ratio between inter and intra-class variances. The present work used a portable infrared spectrometer (NIR) for identification and classification of pure and fiber-fortified semolina samples. The fiber was added to semolina in two different concentrations, and after the spectra acquisition, the data was used for PCA and LDA to identify and discriminate the samples. The results showed that NIR spectroscopy associate to PCA was very effective in identifying pure and fiber-fortified semolina. Additionally, the classification range of the samples using LDA was between 78.3% and 95% for calibration and 75% and 95% for cross-validation. Thus, after the multivariate analysis such as PCA and LDA, it was possible to verify that NIR associated to chemometric methods is able to identify and classify the different samples in a fast and non-destructive way.

Keywords: Chemometrics, fiber, linear discriminant analysis, near-infrared spectroscopy, principal component analysis, semolina

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Authors: S. Mohammadzamani, B. Kordi

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Wireless electric field sensors are in high demand in the number of applications that requires measuring electric field such as investigations of high power systems and testing the high voltage apparatus. Passive wireless electric field sensors are most desired since they do not require a source of power and are interrogated wirelessly. A passive wireless electric field sensor has been designed and fabricated by our research group. In the wireless interrogation system of the sensor, a wireless radio frequency impulse generator needs to be employed. A compact wireless impulse generator composed of an integrated resonant switched oscillator (SWO) and a pulse-radiating antenna has been designed and fabricated in this research. The fundamental of Switched Oscillators was introduced by C.E.Baum. A Switched Oscillator consists of a low impedance transmission line charged by a DC source, through large impedance at desired frequencies and terminated to a high impedance antenna at one end and a fast closing switch at the other end. Once the line is charged, the switch will close and short-circuit the transmission line. Therefore, a fast transient wave will be generated and travels along the transmission line. Because of the mismatch between the antenna and the transmission line, only a part of fast transient wave will be radiated, and a portion of the fast-transient wave will reflect back. At the other end of the transmission line, there is a closed switch. Consequently, a second reflection with a reversed sign will propagate towards the antenna and the wave continues back and forth. hence, at the terminal of the antenna, there will be a series of positive and negative pulses with descending amplitude. In this research a single ended quarter wavelength Switched Oscillator has been designed and simulated at 800MHz. The simulation results show that the designed Switched Oscillator generates pulses with decreasing amplitude at the frequency of 800MHz with the maximum amplitude of 10V and bandwidth of about 10MHz at the antenna end. The switched oscillator has been fabricated using a 6cm long coaxial cable transmission line which is charged by a DC source and an 8cm monopole antenna as the pulse radiating antenna. A 90V gas discharge switch has been employed as the fast closing switch. The Switched oscillator sends a series of pulses with decreasing amplitude at the frequency of 790MHz with the maximum amplitude of 0.3V in the distance of 30 cm.

Keywords: electric field measurement, impulse radiating antenna, switched oscillator, wireless impulse generator

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Authors: Marta Chiapasco, Alexandra Porter, Finn Giuliani

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Designing polymers with a specific microstructure can affect how the polymer degrades once released in the environment. Not only the amount but also the distribution of different phases determines a polymers’ degradability. The following research investigates the use of a combination of spectroscopy analysis and thermal analysis to study changes of polymers’ amorphous and crystalline phases during degradation, comparing different microstructures of polypropylene and polyethylene. The use of nanoindentation helps study how degradation proceeds across a material by looking at changes in phases, while bulk tensile test describes when the material fails. The first results demonstrate that different microstructures have different degrading rates, with homopolymer having a linear and faster degradation compared to copolymers. The goal is to create materials that degrade at faster rates without releasing microplastics into the environment.

Keywords: degradation, microstructure, nanoindentation, Raman spectroscopy

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Authors: Chen-Fu Wang, Lin-Ya Kung

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For traditional painting materials, the artisan used to combine the pigments with different binders to create colors. As time goes by, the materials used for painting evolved from natural to chemical materials. The vast variety of ingredients used in chemical materials has complicated restoration work; it makes conservation work more difficult. Conservation work also becomes harder when the materials cannot be easily identified; therefore, it is essential that we take a more scientific approach to assist in conservation work. Paintings materials are high molecular weight polymer, and their analysis is very complicated as well other contamination such as smoke and dirt can also interfere with the analysis of the material. The current methods of composition analysis of painting materials include Fourier transform infrared spectroscopy (FT-IR), mass spectrometer, Raman spectroscopy, X-ray diffraction spectroscopy (XRD), each of which has its own limitation. In this study, FT-IR was used to analyze the components of the paint coating. We have taken the most commonly seen materials as samples and deteriorated it. The aged information was then used for the database to exam the temple painting materials. By observing the FT-IR changes over time, we can tell all of the painting materials will be deteriorated by the UV light, but only the speed of its degradation had some difference. From the deterioration experiment, the acrylic resin resists better than the others. After collecting the painting materials aging information on FT-IR, we performed some test on the paintings on the temples. It was found that most of the artisan used tune-oil for painting materials, and some other paintings used chemical materials. This method is now working successfully on identifying the painting materials. However, the method is destructive and high cost. In the future, we will work on the how to know the painting materials more efficiently.

Keywords: temple painting, painting material, conservation, FT-IR

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Authors: Angelo Gabriel Buenaventura, Allan Christopher Yago

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A carbon paste electrode (CPE) composed of Multiwalled Carbon Nanotube (MWCNT) conducting particle and Polydimethylsiloxane (PDMS) binder was used for simultaneous detection of Dopamine (DA) and Uric Acid (UA) in the presence of Ascorbic Acid (AA) at physiological level. The MWCNT-PDMS CPE was initially activated via potentiodynamic cycling in a basic (NaOH) solution, which resulted in enhanced electrochemical properties. Electrochemical Impedance Spectroscopy measurements revealed a significantly lower charge transfer resistance (Rct) for the OH--activated MWCNT-PDMS CPE (Rct = 5.08kΩ) as compared to buffer (pH 7)-activated MWCNT-PDMS CPE (Rct = 25.9kΩ). Reversibility analysis of Fe(CN)63-/4- redox couple of both Buffer-Activated CPE and OH--Activated CPE showed that the OH—Activated CPE have peak current ratio (Ia/Ic) of 1.11 at 100mV/s while 2.12 for the Buffer-Activated CPE; this showed an electrochemically reversible behavior for Fe(CN)63-/4- redox couple even at relatively fast scan rate using the OH--activated CPE. Enhanced voltammetric signal for DA and significant peak separation between DA and UA was obtained using the OH--activated MWCNT-PDMS CPE in the presence of 50 μM AA via Differential Pulse Voltammetry technique. The anodic peak currents which appeared at 0.263V and 0.414 V were linearly increasing with increasing concentrations of DA and UA, respectively. The linear ranges were obtained at 25 μM – 100 μM for both DA and UA. The detection limit was determined to be 3.86 μM for DA and 5.61 μM for UA. These results indicate a practical approach in the simultaneous detection of important bio-organic molecules using a simple CPE composed of MWCNT and PDMS with base anodization as activation technique.

Keywords: anodization, ascorbic acid, carbon paste electrodes, dopamine, uric acid

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Authors: Duygu Çimen, Nilay Bereli, Adil Denizli

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In this study is to synthesis magnetic nanoparticles for purify protein C. For this aim, N-Methacryloyl-(L)-histidine methyl ester (MAH) containing 2-hydroxyethyl methacrylate (HEMA) based magnetic nanoparticles were synthesized by using micro-emulsion polymerization technique for templating protein C via metal chelation. The obtained nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), zeta-size analysis and electron spin resonance (ESR) spectroscopy. After that, they were used for protein C purification from aqueous solution to evaluate/optimize the adsorption condition. Hereby, the effecting factors such as concentration, pH, ionic strength, temperature, and reusability were evaluated. As the last step, protein C was determined with sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Keywords: immobilized metal affinity chromatography (IMAC), magnetic nanoparticle, protein C, hydroxyethyl methacrylate (HEMA)

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Authors: S. K. M. Nzaba, H. H. Nyoni, B. Ntsendwana, B. B. Mamba, A. T. Kuvarega

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Azo dye effluents, released into water bodies are not only toxic to the ecosystem but also pose a serious impact on human health due to the carcinogenic and mutagenic effects of the compounds present in the dye discharge. Conventional water treatment methods such as adsorption, flocculation/coagulation and biological processes are not effective in completely removing most of the dyes and their natural degradation by-products. Advanced oxidation processes (AOPs) have proven to be effective technologies for complete mineralization of these recalcitrant pollutants. Therefore, there is a need for new technology that can solve the problem. Thus, this study examined the photocatalytic degradation of an azo dye brilliant black (BB) using non-metal/metal codoped TiO₂. N, Pt co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine-terminated polyamidoamine dendrimer generation 0 (PAMAM G0), amine-terminated polyamidoamine dendrimer generation 1 ( PAMAM G1) and hyperbranched polyethyleneimine (HPEI) as templates and source of nitrogen. Structural, morphological, and textural properties were evaluated using scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (SEM/EDX), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), Fourier- transform infrared (FTIR), Raman spectroscopy (RS), photoluminescence (PL) and ultra-violet /visible spectroscopy (UV-Vis). The synthesized photocatalysts exhibited lower band gap energies as compared to the Degussa P-25 revealing a red shift in band gap towards the visible light absorption region. Photocatalytic activity of N, Pt co-doped TiO₂ was measured by the reaction of photocatalytic degradation of brilliant black (BB) dye. The N, metal codoped TiO₂ containing 0.5 wt. % of the metal consisted mainly of the anatase phase as confirmed by XRD results of all three samples, with a particle size range of 13–30 nm. The particles were largely spherical and shifted the absorption edge well into the visible region. Band gap reduction was more pronounced for the N, Pt HPEI (Pt 0.5 wt. %) codoped TiO₂ compared to PAMAM G0 and PAMAM G1. Consequently, codoping led to an enhancement in the photocatalytic activity of the materials for the degradation of brilliant black (BB).

Keywords: codoped TiO₂, dendrimer, photodegradation, wastewater

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Authors: Natsumi Murakami, Jae-Ho Kim, Susumu Yonezawa

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The calcium fluorosilicate (CaSiF₆) was prepared from calcium silicate (CaSiO₃) with fluorine gas at 25 ~ 200 ℃ and 760 Torr for 1~24 h. Especially, the pure CaSiF₆ could be prepared at 25 ℃ for 24 h with F₂ gas from the results of X-ray diffraction. Increasing temperature to higher than 100 ℃, the prepared CaSiF₆ was decomposed into CaF₂ and SiF₄. The release of SiF₄ gas was confirmed by the results of gas-phase infrared spectroscopy. In this study, we tried to modify the surface of polycarbonate (PC) resin using the SiF₄ gas released from CaSiF₆ particles. By using the prepared CaSiF₆, the surface roughness of fluorinated PC samples was approximately four times larger than that (1.4 nm) of the untreated sample. The results of X-ray photoelectron spectroscopy indicated the formation of fluorinated bonds (e.g., -CFx) on the surface of PC after surface fluorination. Consequently, the CaSiF₆ particles can be useful for a new fluorinating agent.

Keywords: calcium fluorosilicate, fluorinating agent, polycarbonate, surface fluorination

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Authors: M. Kalbac, T. Verhagen, K. Drogowska, J. Vejpravova

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One- and two-dimensional carbon nano structures with sp2 hybridization of carbon atoms (single walled carbon nano tubes and graphene) are promising materials in future electronic and spintronics devices due to specific character of their electronic structure. In this paper, we present a comparative study of graphene and single-wall carbon nano tubes by Raman spectro-microscopy in strong magnetic field. This unique method allows to study changes in electronic band structure of the two types of carbon nano structures induced by a strong magnetic field.

Keywords: carbon nano structures, magnetic field, raman spectroscopy, spectro-microscopy

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Authors: R. Buntem, K. Samkongngam

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The silicate glass was prepared using rice husk as the source of silica. The base composition of glass sample is composed of SiO2 (from rice husk ash), Na2CO3, K2CO3, ZnO, H3BO3, CaO, Al2O3 or Al, and CuO. Aluminum is used in place of Al2O3 in order to reduce Cu2+ to Cu+. The red color of Cu2O in the glass matrix was observed when the Al was added into the glass mixture. The expansion coefficients of the copper doped glass are in the range of 1.2 x 10-5-1.4x10-5 (ºC -1) which is common for the silicate glass. The finger prints of the bond vibrations were studied using IR spectroscopy. While the oxidation state and the coordination information of the copper ion in the glass matrix were investigated using X-ray absorption spectroscopy. From the data, Cu+ and Cu2+ exist in the glass matrix. The red particles of Cu2O can be formed in the glass matrix when enough aluminum was added.

Keywords: copper in glass, coordination information, silicate glass, XANES spectrum

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Authors: Irmak Gunes Yuceil

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This paper outlines interferences and analytical errors which are encountered in the qualification and quantification of archaeological and ethnographic artifacts, by means of handheld x-ray fluorescence. These shortcomings were evaluated through case studies carried out on metallic artifacts related to various periods and cultures around Anatolia. An Innov-X Delta Standard 2000 handheld x-ray fluorescence spectrometer was used to collect data from 1361 artifacts, through 6789 measurements and 70 hours’ tube usage, in between 2013-2017. Spectrum processing was done by Delta Advanced PC Software. Qualitative and quantitative results screened by the device were compared with the spectrum graphs, and major discrepancies associated with physical and analytical interferences were clarified in this paper.

Keywords: hand-held x-ray fluorescence spectroscopy, art and archaeology, interferences and analytical errors, pre-diagnosis in conservation

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Authors: Rajnish Shrivastava, Y. R. Sood, Priti Pundir, Rahul Srivastava

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Power transformer is one of the most important devices that are used in power station. Due to several fault impending upon it or due to ageing, etc its life gets lowered. So, it becomes necessary to have diagnosis of oil for fault analysis. Due to the chemical, electrical, thermal and mechanical stress the insulating material in the power transformer degraded. It is important to regularly assess the condition of oil and the remaining life of the power transformer. In this paper UV-VIS absorption graph area is correlated with moisture content, Flash point, IFT and Density of Transformer oil. Since UV-VIS absorption graph area varies accordingly with the variation in different transformer parameters. So by obtaining the correlation among different oil parameters for oil with respect to UV-VIS absorption area, decay contents of transformer oil can be predicted

Keywords: breakdown voltage (BDV), interfacial Tension (IFT), moisture content, ultra violet-visible rays spectroscopy (UV-VIS)

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Authors: Sultan Ben Jaber

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Optical properties of molecules exhibit dramatic changes when adsorbed close to nano-structure metallic surfaces such as gold and silver nanomaterial. This phenomena opened a wide range of research to improve conventional spectroscopies efficiency. A well-known technique that has an intensive focus of study is surface-enhanced Raman spectroscopy (SERS), as since the first observation of SERS phenomena, researchers have published a great number of articles about the potential mechanisms behind this effect as well as developing materials to maximize the enhancement. Infrared and Raman spectroscopy are complementary techniques; thus, surface-enhanced infrared absorption (SEIRA) also shows a noticeable enhancement of molecules in the mid-IR excitation on nonmetallic structure substrates. In the SEIRA, vibrational modes that gave change in dipole moments perpendicular to the nano-metallic substrate enhanced 200 times greater than the free molecule’s modes. SEIRA spectroscopy is promising for the characterization and identification of adsorbed molecules on metallic surfaces, especially at trace levels. IR reflection-absorption spectroscopy (IRAS) is a well-known technique for measuring IR spectra of adsorbed molecules on metallic surfaces. However, SEIRA spectroscopy sensitivity is up to 50 times higher than IRAS. SEIRA enhancement has been observed for a wide range of molecules adsorbed on metallic substrates such as Au, Ag, Pd, Pt, Al, and Ni, but Au and Ag substrates exhibited the highest enhancement among the other mentioned substrates. In this work, trace levels of 3,4-methylenedioxymethamphetamine (MDMA) have been detected using gold nanoparticles (AuNPs) substrates with surface-enhanced infrared absorption (SEIRA). AuNPs were first prepared and washed, then mixed with different concentrations of MDMA samples. The process of fabricating the substrate prior SEIRA measurements included mixing of AuNPs and MDMA samples followed by vigorous stirring. The stirring step is particularly crucial, as stirring allows molecules to be robustly adsorbed on AuNPs. Thus, remarkable SEIRA was observed for MDMA samples even at trace levels, showing the rigidity of our approach to preparing SEIRA substrates.

Keywords: surface-enhanced infrared absorption (SEIRA), gold nanoparticles (AuNPs), amphetamines, methylene dioxy- methamphetamine (MDMA), enhancement factor

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Authors: Hadjer Didouh, Izzaddine Sameut Bouhaik, Mohammed Hadj Meliani

Abstract:

This research delves into the intricate dynamics of biofilm adhesion on surfaces, particularly focusing on the widely employed X52 surface in oil and gas industry pipelines. Biofilms, characterized by microorganisms within a self-produced matrix, pose significant challenges due to their detrimental impact on surfaces. Our study integrates advanced molecular techniques and cutting-edge microscopy, such as scanning electron microscopy (SEM), to identify microbial communities and visually assess biofilm adhesion. Simultaneously, we concentrate on the X52 surface, utilizing impedance spectroscopy and potentiodynamic polarization to gather electrochemical responses under various conditions. In conjunction with the broader investigation, we propose a novel approach to mitigate biofilm-induced corrosion challenges. This involves environmentally friendly inhibitors derived from plants, offering a sustainable alternative to conventional chemical treatments. Our inquiry screens and selects inhibitors based on their efficacy in hindering biofilm formation and reducing corrosion rates on the X52 surface. This study contributes valuable insights into the interplay between electrochemical processes and biofilm attachment on the X52 surface. Furthermore, the outcomes of this research have broader implications for the oil and gas industry, where biofilm-related corrosion is a persistent concern. The exploration of eco-friendly inhibitors not only holds promise for corrosion control but also aligns with environmental considerations and sustainability goals. The comprehensive nature of this research aims to enhance our understanding of biofilm dynamics, provide effective strategies for corrosion mitigation, and contribute to sustainable practices in pipeline management within the oil and gas sector.

Keywords: bio-corrosion, biofilm, attachment, X52, metal/bacteria interface

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Authors: Nader Nciri, Suil Song, Namho Kim, Namjun Cho

Abstract:

Properties and compositions of bitumen and bitumen-derived liquids have significant influences on the selection of recovery, upgrading and refining processes. Optimal process conditions can often be directly related to these properties. The end uses of bitumen and bitumen products are thus related to their compositions. Because it is not possible to conduct a complete analysis of the molecular structure of bitumen, characterization must be made in other terms. The present paper focuses on physico-chemical analysis of two different types of bitumens. These bitumen samples were chosen based on: the original crude oil (sand oil and crude petroleum), and mode of process. The aim of this study is to determine both the manufacturing effect on chemical species and the chemical organization as a function of the type of bitumen sample. In order to obtain information on bitumen chemistry, elemental analysis (C, H, N, S, and O), heavy metal (Ni, V) concentrations, IATROSCAN chromatography (thin layer chromatography-flame ionization detection), FTIR spectroscopy, and 1H NMR spectroscopy have all been used. The characterization includes information about the major compound types (saturates, aromatics, resins and asphaltenes) which can be compared with similar data for other bitumens, more importantly, can be correlated with data from petroleum samples for which refining characteristics are known. Examination of Asphalt Ridge froth bitumen showed that it differed significantly from representative petroleum pitches, principally in their nonhydrocarbon content, heavy metal content and aromatic compounds. When possible, properties and composition were related to recovery and refining processes. This information is important because of the effects that composition has on recovery and processing reactions.

Keywords: froth bitumen, oil sand, asphalt ridge, petroleum pitch, thin layer chromatography-flame ionization detection, infrared spectroscopy, 1H nuclear magnetic resonance spectroscopy

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Authors: Yingjeng James Li, Yun Jyun Ou, Chih Chi Hsu, Chiao-Chih Hu

Abstract:

A fuel cell is a device that produces electric power by reacting fuel and oxidant electrochemically. There is no pollution produced from a fuel cell if hydrogen is employed as the fuel. Therefore, a fuel cell is considered as a zero emission device and is a source of green power. A membrane electrode assembly (MEA) is the key component of a fuel cell. It is, therefore, beneficial to develop MEAs with high performance. In this study, an MEA for proton exchange membrane fuel cell (PEMFC) was prepared from a 15-micron thick reinforced PEM. The active area of such MEA is 25 cm2. Carbon supported platinum (Pt/C) was employed as the catalyst for both anode and cathode. The platinum loading is 0.6 mg/cm2 based on the sum of anode and cathode. Commercially available carbon papers coated with a micro porous layer (MPL) serve as gas diffusion layers (GDLs). The original thickness of the GDL is 250 μm. It was compressed down to 163 μm when assembled into the single cell test fixture. Polarization curves were taken by using eight different test conditions. At our standard test condition (cell: 70 °C; anode: pure hydrogen, 100%RH, 1.2 stoic, ambient pressure; cathode: air, 100%RH, 3.0 stoic, ambient pressure), the cell current density is 1250 mA/cm2 at 0.6 V, and 2400 mA/cm2 at 0.4 V. At self-humidified condition and cell temperature of 55 °C, the cell current density is 1050 mA/cm2 at 0.6 V, and 2250 mA/cm2 at 0.4 V. Hydrogen crossover rate of the MEA is 0.0108 mL/min*cm2 according to linear sweep voltammetry experiments. According to the MEA’s Pt loading and the cyclic voltammetry experiments, the Pt electrochemical surface area is 60 m2/g. The ohmic part of the impedance spectroscopy results shows that the membrane resistance is about 60 mΩ*cm2 when the MEA is operated at 0.6 V.

Keywords: fuel cell, membrane electrode assembly, proton exchange membrane, reinforced

Procedia PDF Downloads 289

Authors: Liping Wu, Durga Bhakta Pokharel, Junhua Dong, Changgang Wang, Lin Zhao, Wei Ke, Nan Chen

Abstract:

Hazenite conversion coating was deposited on AZ31 Mg alloy in a deaerated phosphate solution containing 0.1 M K₂HPO₄ and 0.1 M Na₂HPO₄ (Na₀.₁K0₀.₁) with pH 9 at −0.8 V. The coating mechanism of hazenite was elucidated by in situ potentiostatic current decay, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), electron probe micro-analyzer (EPMA) and differential scanning calorimetry (DSC). The volume of H₂ evolved during potentiostatic polarization was measured by a gas collection apparatus. The degradation resistance of the hazenite coating was evaluated in simulated body fluid (SBF) at 37℃ by using potentiodynamic polarization (PDP). The results showed that amorphous Mg(OH)₂ was deposited first, followed by the transformation of Mg(OH)₂ to amorphous MgHPO₄, subsequently the conversion of MgHPO₄ to crystallized K-struvite (KMgPO₄·6H₂O), finally the crystallization of crystallized hazenite (NaKMg₂(PO₄)₂·14H₂O). The deposited coating was composed of four layers where the inner layer is comprised of Mg(OH)₂, the middle layer of Mg(OH)₂ and MgHPO₄, the top layer of Mg(OH)₂, MgHPO₄ and K-struvite, the topmost layer of Mg(OH)₂, MgHPO₄, K-struvite and hazenite (NaKMg₂(PO₄)₂·14H₂O). The PD results showed that the hazenite coating decreased the corrosion rate by two orders of magnitude.

Keywords: magnesium alloy, potentiostatic technique, hazenite, mineral conversion coating

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Authors: V. Pizarro-Carmona, S. Castano-Solis, M. Cortés-Carmona, J. Fraile-Ardanuy, D. Jimenez-Bermejo

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The purpose of this article is to optimize the Equivalent Electric Circuit Model (EECM) of different orders to obtain greater precision in the modeling of Li-ion battery packs. Optimization includes considering circuits based on 1RC, 2RC and 3RC networks, with a dependent voltage source and a series resistor. The parameters are obtained experimentally using tests in the time domain and in the frequency domain. Due to the high non-linearity of the behavior of the battery pack, Genetic Algorithm (GA) was used to solve and optimize the parameters of each EECM considered (1RC, 2RC and 3RC). The objective of the estimation is to minimize the mean square error between the measured impedance in the real battery pack and those generated by the simulation of different proposed circuit models. The results have been verified by comparing the Nyquist graphs of the estimation of the complex impedance of the pack. As a result of the optimization, the 2RC and 3RC circuit alternatives are considered as viable to represent the battery behavior. These battery pack models are experimentally validated using a hardware-in-the-loop (HIL) simulation platform that reproduces the well-known New York City cycle (NYCC) and Federal Test Procedure (FTP) driving cycles for electric vehicles. The results show that using GA optimization allows obtaining EECs with 2RC or 3RC networks, with high precision to represent the dynamic behavior of a battery pack in vehicular applications.

Keywords: Li-ion battery packs modeling optimized, EECM, GA, electric vehicle applications

Procedia PDF Downloads 118

Authors: Hadjer Didouh, Mohamed Hadj Meliani, Izzeddine Sameut Bouhaik

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As global demand for natural gas intensifies, Algeria is increasing its production to meet this rising need, placing significant strain on the nation's extensive pipeline infrastructure. Sonatrach, Algeria's national oil and gas company, faces persistent challenges from metal corrosion, particularly microbiologically influenced corrosion (MIC), leading to substantial economic losses. This study investigates the corrosion-inhibiting properties of Calotropis procera extracts, known as karanka, as a sustainable alternative to conventional inhibitors, which often pose environmental risks. The Calotropis procera extracts were evaluated for their efficacy on carbon steel API 5L X52 through electrochemical techniques, including potentiodynamic polarization and electrochemical impedance spectroscopy (EIS), under simulated operational conditions at varying concentrations, particularly at 10%, and elevated temperatures up to 60°C. The results demonstrated remarkable inhibition efficiency, achieving 96.73% at 60°C, attributed to the formation of a stable protective film on the metal surface that suppressed anodic and cathodic corrosion reactions. Scanning electron microscopy (SEM) confirmed the stability and adherence of these protective films, while EIS analysis indicated a significant increase in charge transfer resistance, highlighting the extract's effectiveness in enhancing corrosion resistance. The abundant availability of Calotropis procera in Algeria and its low-cost extraction processes present a promising opportunity for sustainable biocorrosion management strategies in the oil and gas industry, reinforcing the potential of plant-based extracts as viable alternatives to synthetic inhibitors for environmentally friendly corrosion control.

Keywords: corrosion inhibition, calotropis procera, microbiologically influenced corrosion, eco-friendly inhibitor

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Authors: Ljerka Kratofil Krehula, Martina Perlog, Jasmina Stjepanović, Vanja Gilja, Marijana Kraljić Roković, Zlata Hrnjak-Murgić

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The composite preparation of titanium dioxide and zinc oxide photocatalysts with the conductive polymers gives the opportunity to carry out the catalysis reactions not only under UV light but also under visible light. Such processes may efficiently use sunlight in degradation of different organic pollutants and present new design for wastewater treatment. The paper presents the preparation procedure, material characteristics and photocatalytic efficiency of polypyrrole/titanium dioxide and polypyrrole/zinc oxide composites (PPy/TiO2 and PPy/ZnO). The obtained composite samples were characterized by Fourier transform infrared spectroscopy (FTIR), UV-Vis spectroscopy and thermogravimetric analysis (TGA). The photocatalytic efficiency of the samples was determined following the decomposition of Acid Blue 25 dye (AB 25) under UV and visible light by UV/Vis spectroscopy. The efficiency of degradation is determined by total organic carbon content (TOC) after photocatalysis processes. The results show enhanced photocatalytic efficiency of the samples under visible light, so the prepared composite samples are recognized as efficient catalysts in degradation process of AB 25 dye. It can be concluded that the preparation of TiO2 or ZnO composites with PPy can serve as a very efficient method for the improvement of TiO2 and ZnO photocatalytic performance under visible light.

Keywords: composite, photocatalysis, polypyrrole, titanium dioxide, zinc oxide

Procedia PDF Downloads 477

Authors: Siti Nurhidayah Naqiah Abdull Rani, Herlina Abdul Rahim

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Near infrared (NIR) spectroscopy has always been of great interest in the food and agriculture industries. The development of predictive models has facilitated the estimation process in recent years. In this research, 176 crude palm oil (CPO) samples acquired from Felda Johor Bulker Sdn Bhd were studied. A FOSS NIRSystem was used to tak e absorbance measurements from the sample. The wavelength range for the spectral measurement is taken at 1600nm to 1900nm. Partial Least Square Regression (PLSR) prediction model with 50 optimal number of principal components was implemented to study the relationship between the measured Free Fatty Acid (FFA) values and the measured spectral absorption. PLSR showed predictive ability of FFA values with correlative coefficient (R) of 0.9808 for the training set and 0.9684 for the testing set.

Keywords: palm oil, fatty acid, NIRS, PLSR

Procedia PDF Downloads 204