Search results for: impedance spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 2181

Search results for: impedance spectroscopy

1851 Nanoparticle Based Green Inhibitor for Corrosion Protection of Zinc in Acidic Medium

Authors: Neha Parekh, Divya Ladha, Poonam Wadhwani, Nisha Shah

Abstract:

Nano scaled materials have attracted tremendous interest as corrosion inhibitor due to their high surface area on the metal surfaces. It is well known that the zinc oxide nanoparticles have higher reactivity towards aqueous acidic solution. This work presents a new method to incorporate zinc oxide nanoparticles with white sesame seeds extract (nano-green inhibitor) for corrosion protection of zinc in acidic medium. The morphology of the zinc oxide nanoparticles was investigated by TEM and DLS. The corrosion inhibition efficiency of the green inhibitor and nano-green inhibitor was determined by Gravimetric and electrochemical impedance spectroscopy (EIS) methods. Gravimetric measurements suggested that nano-green inhibitor is more effective than green inhibitor. Furthermore, with the increasing temperature, inhibition efficiency increases for both the inhibitors. In addition, it was established the Temkin adsorption isotherm fits well with the experimental data for both the inhibitors. The effect of temperature and Temkin adsorption isotherm revealed Chemisorption mechanism occurring in the system. The activation energy (Ea) and other thermodynamic parameters for inhibition process were calculated. The data of EIS showed that the charge transfer controls the corrosion process. The surface morphology of zinc metal (specimen) in absence and presence of green inhibitor and nano-green inhibitor were performed using Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) techniques. The outcomes indicated a formation of a protective layer over zinc metal (specimen).

Keywords: corrosion, green inhibitor, nanoparticles, zinc

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1850 Analytical Authentication of Butter Using Fourier Transform Infrared Spectroscopy Coupled with Chemometrics

Authors: M. Bodner, M. Scampicchio

Abstract:

Fourier Transform Infrared (FT-IR) spectroscopy coupled with chemometrics was used to distinguish between butter samples and non-butter samples. Further, quantification of the content of margarine in adulterated butter samples was investigated. Fingerprinting region (1400-800 cm–1) was used to develop unsupervised pattern recognition (Principal Component Analysis, PCA), supervised modeling (Soft Independent Modelling by Class Analogy, SIMCA), classification (Partial Least Squares Discriminant Analysis, PLS-DA) and regression (Partial Least Squares Regression, PLS-R) models. PCA of the fingerprinting region shows a clustering of the two sample types. All samples were classified in their rightful class by SIMCA approach; however, nine adulterated samples (between 1% and 30% w/w of margarine) were classified as belonging both at the butter class and at the non-butter one. In the two-class PLS-DA model’s (R2 = 0.73, RMSEP, Root Mean Square Error of Prediction = 0.26% w/w) sensitivity was 71.4% and Positive Predictive Value (PPV) 100%. Its threshold was calculated at 7% w/w of margarine in adulterated butter samples. Finally, PLS-R model (R2 = 0.84, RMSEP = 16.54%) was developed. PLS-DA was a suitable classification tool and PLS-R a proper quantification approach. Results demonstrate that FT-IR spectroscopy combined with PLS-R can be used as a rapid, simple and safe method to identify pure butter samples from adulterated ones and to determine the grade of adulteration of margarine in butter samples.

Keywords: adulterated butter, margarine, PCA, PLS-DA, PLS-R, SIMCA

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1849 Synthesis and Characterization of CNPs Coated Carbon Nanorods for Cd2+ Ion Adsorption from Industrial Waste Water and Reusable for Latent Fingerprint Detection

Authors: Bienvenu Gael Fouda Mbanga

Abstract:

This study reports a new approach of preparation of carbon nanoparticles coated cerium oxide nanorods (CNPs/CeONRs) nanocomposite and reusing the spent adsorbent of Cd2+- CNPs/CeONRs nanocomposite for latent fingerprint detection (LFP) after removing Cd2+ ions from aqueous solution. CNPs/CeONRs nanocomposite was prepared by using CNPs and CeONRs with adsorption processes. The prepared nanocomposite was then characterized by using UV-visible spectroscopy (UV-visible), Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction pattern (XRD), scanning electron microscope (SEM), Transmission electron microscopy (TEM), Energy-dispersive X-ray spectroscopy (EDS), Zeta potential, X-ray photoelectron spectroscopy (XPS). The average size of the CNPs was 7.84nm. The synthesized CNPs/CeONRs nanocomposite has proven to be a good adsorbent for Cd2+ removal from water with optimum pH 8, dosage 0. 5 g / L. The results were best described by the Langmuir model, which indicated a linear fit (R2 = 0.8539-0.9969). The adsorption capacity of CNPs/CeONRs nanocomposite showed the best removal of Cd2+ ions with qm = (32.28-59.92 mg/g), when compared to previous reports. This adsorption followed pseudo-second order kinetics and intra particle diffusion processes. ∆G and ∆H values indicated spontaneity at high temperature (40oC) and the endothermic nature of the adsorption process. CNPs/CeONRs nanocomposite therefore showed potential as an effective adsorbent. Furthermore, the metal loaded on the adsorbent Cd2+- CNPs/CeONRs has proven to be sensitive and selective for LFP detection on various porous substrates. Hence Cd2+-CNPs/CeONRs nanocomposite can be reused as a good fingerprint labelling agent in LFP detection so as to avoid secondary environmental pollution by disposal of the spent adsorbent.

Keywords: Cd2+-CNPs/CeONRs nanocomposite, cadmium adsorption, isotherm, kinetics, thermodynamics, reusable for latent fingerprint detection

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1848 Ultrasonic Spectroscopy of Polymer Based PVDF-TrFE Composites with CNT Fillers

Authors: J. Belovickis, V. Samulionis, J. Banys, M. V. Silibin, A. V. Solnyshkin, A. V. Sysa

Abstract:

Ferroelectric polymers exhibit good flexibility, processability and low cost of production. Doping of ferroelectric polymers with nanofillers may modify its dielectric, elastic or piezoelectric properties. Carbon nanotubes are one of the ingredients that can improve the mechanical properties of polymer based composites. In this work, we report on both the ultrasonic and the dielectric properties of the copolymer polyvinylidene fluoride/tetrafluoroethylene (P(VDF-TrFE)) of the composition 70/30 mol% with various concentrations of carbon nanotubes (CNT). Experimental study of ultrasonic wave attenuation and velocity in these composites has been performed over wide temperature range (100 K – 410 K) using an ultrasonic automatic pulse-echo tecnique. The temperature dependences of ultrasonic velocity and attenuation showed anomalies attributed to the glass transition and paraelectric-ferroelectric phase transition. Our investigations showed mechanical losses to be dependent on the volume fraction of the CNTs within the composites. The existence of broad hysteresis of the ultrasonic wave attenuation and velocity within the nanocomposites is presented between cooling and heating cycles. By the means of dielectric spectroscopy, it is shown that the dielectric properties may be tuned by varying the volume fraction of the CNT fillers.

Keywords: carbon nanotubes, polymer composites, PVDF-TrFE, ultrasonic spectroscopy

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1847 Synthesis, Characterization and Applications of Some Selected Dye-Functionalized P and N-Type Nanoparticles in Dye Sensitized Solar Cells

Authors: Arifa Batool, Ghulam Hussain Bhatti, Syed Mujtaba Shah

Abstract:

Inorganic n-type (TiO2, CdO) and p-type (NiO, CuO) metal oxide nanoparticles were synthesized by a facile wet chemical method at room temperature. The morphological, compositional, structural and optical properties were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, FT-IR, XRD analysis, UV/Visible and fluorescence spectroscopy. All semiconducting nanoparticles were photosensitized with Ru (II) based Z907 dye in ethanol solvent by grafting. Grafting of dye on the surface of nanoparticles was confirmed by UV/Visible and FT-IR spectroscopy. The synthesized photo-active nanohybrid was thoroughly blended with P3HT, a solid electrolyte and I-V measurements under solar stimulated radiations 1000 W/m2 (AM 1.5) were recorded. Maximum incident photon to current conversion efficiency (IPCE) of 0.9% was achieved with dye functionalized Z907-TiO2 hybrid, IPCE of 0.72% was achieved with bulk-heterojunction of TiO2-Z907-CuO and IPCE of 0.68% was attained with nanocomposite of TiO2-CdO. TiO2 based Solar cells have maximum Jscvalue i.e.4.63 mA/cm2. Dye-functionalized TiO2-based photovoltaic devices were found more efficient than the reference device but the morphology of the device was a major check in progress.

Keywords: solar cell, bulk heterojunction, nanocomposites, photosensitization, dye sensitized solar cell

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1846 Diffusion Magnetic Resonance Imaging and Magnetic Resonance Spectroscopy in Detecting Malignancy in Maxillofacial Lesions

Authors: Mohamed Khalifa Zayet, Salma Belal Eiid, Mushira Mohamed Dahaba

Abstract:

Introduction: Malignant tumors may not be easily detected by traditional radiographic techniques especially in an anatomically complex area like maxillofacial region. At the same time, the advent of biological functional MRI was a significant footstep in the diagnostic imaging field. Objective: The purpose of this study was to define the malignant metabolic profile of maxillofacial lesions using diffusion MRI and magnetic resonance spectroscopy, as adjunctive aids for diagnosing of such lesions. Subjects and Methods: Twenty-one patients with twenty-two lesions were enrolled in this study. Both morphological and functional MRI scans were performed, where T1, T2 weighted images, diffusion-weighted MRI with four apparent diffusion coefficient (ADC) maps were constructed for analysis, and magnetic resonance spectroscopy with qualitative and semi-quantitative analyses of choline and lactate peaks were applied. Then, all patients underwent incisional or excisional biopsies within two weeks from MR scans. Results: Statistical analysis revealed that not all the parameters had the same diagnostic performance, where lactate had the highest areas under the curve (AUC) of 0.9 and choline was the lowest with insignificant diagnostic value. The best cut-off value suggested for lactate was 0.125, where any lesion above this value is supposed to be malignant with 90 % sensitivity and 83.3 % specificity. Despite that ADC maps had comparable AUCs still, the statistical measure that had the final say was the interpretation of likelihood ratio. As expected, lactate again showed the best combination of positive and negative likelihood ratios, whereas for the maps, ADC map with 500 and 1000 b-values showed the best realistic combination of likelihood ratios, however, with lower sensitivity and specificity than lactate. Conclusion: Diffusion weighted imaging and magnetic resonance spectroscopy are state-of-art in the diagnostic arena and they manifested themselves as key players in the differentiation process of orofacial tumors. The complete biological profile of malignancy can be decoded as low ADC values, high choline and/or high lactate, whereas that of benign entities can be translated as high ADC values, low choline and no lactate.

Keywords: diffusion magnetic resonance imaging, magnetic resonance spectroscopy, malignant tumors, maxillofacial

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1845 Atomic Layer Deposition Of Metal Oxide Inverse Opals: A Promising Strategy For Photocatalytic Applications

Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

Abstract:

Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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1844 Kohonen Self-Organizing Maps as a New Method for Determination of Salt Composition of Multi-Component Solutions

Authors: Sergey A. Burikov, Tatiana A. Dolenko, Kirill A. Gushchin, Sergey A. Dolenko

Abstract:

The paper presents the results of clusterization by Kohonen self-organizing maps (SOM) applied for analysis of array of Raman spectra of multi-component solutions of inorganic salts, for determination of types of salts present in the solution. It is demonstrated that use of SOM is a promising method for solution of clusterization and classification problems in spectroscopy of multi-component objects, as attributing a pattern to some cluster may be used for recognition of component composition of the object.

Keywords: Kohonen self-organizing maps, clusterization, multi-component solutions, Raman spectroscopy

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1843 A Non-Invasive Blood Glucose Monitoring System Using near-Infrared Spectroscopy with Remote Data Logging

Authors: Bodhayan Nandi, Shubhajit Roy Chowdhury

Abstract:

This paper presents the development of a portable blood glucose monitoring device based on Near-Infrared Spectroscopy. The system supports Internet connectivity through WiFi and uploads the time series data of glucose concentration of patients to a server. In addition, the server is given sufficient intelligence to predict the future pathophysiological state of a patient given the current and past pathophysiological data. This will enable to prognosticate the approaching critical condition of the patient much before the critical condition actually occurs.The server hosts web applications to allow authorized users to monitor the data remotely.

Keywords: non invasive, blood glucose concentration, microcontroller, IoT, application server, database server

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1842 Statistical Discrimination of Blue Ballpoint Pen Inks by Diamond Attenuated Total Reflectance (ATR) FTIR

Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

Abstract:

Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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1841 A Comparative Analysis of Traditional and Advanced Methods in Evaluating Anti-corrosion Performance of Sacrificial and Barrier Coatings

Authors: Kazem Sabet-Bokati, Ilia Rodionov, Marciel Gaier, Kevin Plucknett

Abstract:

Protective coatings play a pivotal role in mitigating corrosion and preserving the integrity of metallic structures exposed to harsh environmental conditions. The diversity of corrosive environments necessitates the development of protective coatings suitable for various conditions. Accurately selecting and interpreting analysis methods is crucial in identifying the most suitable protective coatings for the various corrosive environments. This study conducted a comprehensive comparative analysis of traditional and advanced methods to assess the anti-corrosion performance of sacrificial and barrier coatings. The protective performance of pure epoxy, zinc-rich epoxy, and cold galvanizing coatings was evaluated using salt spray tests, together with electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization methods. The performance of each coating was thoroughly differentiated under both atmospheric and immersion conditions. The distinct protective performance of each coating against atmospheric corrosion was assessed using traditional standard methods. Additionally, the electrochemical responses of these coatings in immersion conditions were systematically studied, and a detailed discussion on interpreting the electrochemical responses is provided. Zinc-rich epoxy and cold galvanizing coatings offer superior anti-corrosion performance against atmospheric corrosion, while the pure epoxy coating excels in immersion conditions.

Keywords: corrosion, barrier coatings, sacrificial coatings, salt-spray, EIS, polarization

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1840 Exposing Latent Fingermarks on Problematic Metal Surfaces Using Time of Flight Secondary Ion Mass Spectroscopy

Authors: Tshaiya Devi Thandauthapani, Adam J. Reeve, Adam S. Long, Ian J. Turner, James S. Sharp

Abstract:

Fingermarks are a crucial form of evidence for identifying a person at a crime scene. However, visualising latent (hidden) fingermarks can be difficult, and the correct choice of techniques is essential to develop and preserve any fingermarks that might be present. Knives, firearms and other metal weapons have proven to be challenging substrates (stainless steel in particular) from which to reliably obtain fingermarks. In this study, time of flight secondary ion mass spectroscopy (ToF-SIMS) was used to image fingermarks on metal surfaces. This technique was compared to a conventional superglue based fuming technique that was accompanied by a series of contrast enhancing dyes (basic yellow 40 (BY40), crystal violet (CV) and Sudan black (SB)) on three different metal surfaces. The conventional techniques showed little to no evidence of fingermarks being present on the metal surfaces after a few days. However, ToF-SIMS images revealed fingermarks on the same and similar substrates with an exceptional level of detail demonstrating clear ridge definition as well as detail about sweat pore position and shape, that persist for over 26 days after deposition when the samples were stored under ambient conditions.

Keywords: conventional techniques, latent fingermarks, metal substrates, time of flight secondary ion mass spectroscopy

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1839 Relative Importance of Different Mitochondrial Components in Maintaining the Barrier Integrity of Retinal Endothelial Cells: Implications for Vascular-associated Retinal Diseases

Authors: Shaimaa Eltanani, Thangal Yumnamcha, Ahmed S. Ibrahim

Abstract:

Purpose: Mitochondria dysfunction is central to breaking the barrier integrity of retinal endothelial cells (RECs) in various blinding eye diseases such as diabetic retinopathy and retinopathy of prematurity. Therefore, we aimed to dissect the role of different mitochondrial components, specifically, those of oxidative phosphorylation (OxPhos), in maintaining the barrier function of RECs. Methods: Electric cell-substrate impedance sensing (ECIS) technology was used to assess in real-time the role of different mitochondrial components in the total impedance (Z) of human RECs (HRECs) and its components; the capacitance (C) and the total resistance (R). HRECs were treated with specific mitochondrial inhibitors that target different steps in OxPhos: Rotenone for complex I; Oligomycin for ATP synthase; and FCCP for uncoupling OxPhos. Furthermore, data were modeled to investigate the effects of these inhibitors on the three parameters that govern the total resistance of cells: cell-cell interactions (Rb), cell-matrix interactions (α), and cell membrane permeability (Cm). Results: Rotenone (1 µM) produced the greatest reduction in the Z, followed by FCCP (1 µM), whereas no reduction in the Z was observed after the treatment with Oligomycin (1 µM). Following this further, we deconvoluted the effect of these inhibitors on Rb, α, and Cm. Firstly, rotenone (1 µM) completely abolished the resistance contribution of Rb, as the Rb became zero immediately after the treatment. Secondly, FCCP (1 µM) eliminated the resistance contribution of Rb only after 2.5 hours and increased Cm without considerable effect on α. Lastly, Oligomycin had the lowest impact among these inhibitors on Rb, which became similar to the control group at the end of the experiment without noticeable effects on Cm or α. Conclusion: These results demonstrate differential roles for complex I, complex V, and coupling of OxPhos in maintaining the barrier functionality of HRECs, in which complex I being the most important component in regulating the barrier functionality and the spreading behavior of HRECs. Such differences can be used in investigating gene expression as well as for screening selective agents that improve the functionality of complex I to be used in the therapeutic approach for treating REC-related retinal diseases.

Keywords: human retinal endothelial cells (hrecs), rotenone, oligomycin, fccp, oxidative phosphorylation, oxphos, capacitance, impedance, ecis modeling, rb resistance, α resistance, and barrier integrity

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1838 X-Ray Diffraction and Mӧssbauer Studies of Nanostructured Ni45Al45Fe10 Powders Elaborated by Mechanical Alloying

Authors: N. Ammouchi

Abstract:

We have studied the effect of milling time on the structural and hyperfine properties of Ni45Al45Fe10 compound elaborated by mechanical alloying. The elaboration was performed by using the planetary ball mill at different milling times. The as milled powders were characterized by X-ray diffraction (XRD) and Mӧssbauer spectroscopy. From XRD diffraction spectra, we show that the β NiAl(Fe) was completely formed after 24 h of milling time. When the milling time increases, the lattice parameter increases, whereas the grain size decreases to a few nanometres and the mean level of microstrains increases. The analysis of Mӧssbauer spectra indicates that, in addition to a ferromagnetic phase, α-Fe, a paramagnetic disordered phase Ni Al (Fe) solid solution is observed after 2h and only this phase is present after 12h.

Keywords: NiAlFe, nanostructured powders, X-ray diffraction, Mӧssbauer spectroscopy

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1837 Carbon Nanofilms on Diamond for All-Carbon Chemical Sensors

Authors: Vivek Kumar, Alexander M. Zaitsev

Abstract:

A study on chemical sensing properties of carbon nanofilms on diamond for developing all-carbon chemical sensors is presented. The films were obtained by high temperature graphitization of diamond followed by successive plasma etchings. Characterization of the films was done by Raman spectroscopy, atomic force microscopy, and electrical measurements. Fast and selective response to common organic vapors as seen as sensitivity of electrical conductance was observed. The phenomenological description of the chemical sensitivity is proposed as a function of the surface and bulk material properties of the films.

Keywords: chemical sensor, carbon nanofilm, graphitization of diamond, plasma etching, Raman spectroscopy, atomic force microscopy

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1836 Low-Temperature Luminescence Spectroscopy of Violet Sr-Al-O:Eu2+ Phosphor Particles

Authors: Keiji Komatsu, Hayato Maruyama, Ariyuki Kato, Atsushi Nakamura, Shigeo Ohshio, Hiroki Akasaka, Hidetoshi Saitoh

Abstract:

Violet Sr–Al–O:Eu2+ phosphor particles were synthesized from a metal–ethylenediaminetetraacetic acid (EDTA) solution of Sr, Al, Eu, and particulate alumina via spray drying and sintering in a reducing atmosphere. The crystal structures and emission properties at 85–300 K were investigated. The composition of the violet Sr–Al–O:Eu2+ phosphor particles was determined from various Sr–Al–O:Eu2+ phosphors by their emission properties’ dependence on temperature. The highly crystalline SrAl12O19:Eu2+ emission phases were confirmed by their crystallite sizes and the activation energies for the 4f5d–8S7/2 transition of the Eu2+ ion. These results showed that the material identification for the violet Sr–Al–O:Eu2+ phosphor was accomplished by the low-temperature luminescence measurements.

Keywords: low temperature luminescence spectroscopy, material identification, strontium aluminates phosphor, emission properties

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1835 Probing Multiple Relaxation Process in Zr-Cu Base Alloy Using Mechanical Spectroscopy

Authors: A. P. Srivastava, D. Srivastava, D. J. Browne

Abstract:

Relaxation dynamics of Zr44Cu40Al8Ag8 bulk metallic glass (BMG) has been probed using dynamic mechanical analyzer. The BMG sample was casted in the form of a plate of dimension 55 mm x 40 mm x 3 mm using tilt casting technique. X-ray diffraction and transmission electron microscope have been used for the microstructural characterization of as-cast BMG. For the mechanical spectroscopy study, samples in the form of a bar of size 55 mm X 2 mm X 3 mm were machined from the BMG plate. The mechanical spectroscopy was performed on dynamic mechanical analyzer (DMA) by 50 mm 3-point bending method in a nitrogen atmosphere. It was observed that two glass transition process were competing in supercooled liquid region around temperature 390°C and 430°C. The supercooled liquid state was completely characterized using DMA and differential scanning calorimeter (DSC). In addition to the main α-relaxation process, presence of β relaxation process around temperature 360°C; below the glass transition temperature was also observed. The β relaxation process could be described by Arrhenius law with the activation energy of 160 kJ/mole. The volume of the flow unit associated with this relaxation process has been estimated. The results from DMA study has been used to characterize the shear transformation zone in terms of activation volume and size. High fragility parameter value of 34 and higher activation volume indicates that this alloy could show good plasticity in supercooled liquid region. The possible mechanism for the relaxation processes has been discussed.

Keywords: DMA, glass transition, metallic glass, thermoplastic forming

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1834 Characterization of Organic Matter in Spodosol Amazonian by Fluorescence Spectroscopy

Authors: Amanda M. Tadini, Houssam Hajjoul, Gustavo Nicolodelli, Stéphane Mounier, Célia R. Montes, Débora M. B. P. Milori

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Soil organic matter (SOM) plays an important role in maintaining soil productivity and accounting for the promotion of biological diversity. The main components of the SOM are the humic substances which can be fractionated according to its solubility in humic acid (HA), fulvic acids (FA) and humin (HU). The determination of the chemical properties of organic matter as well as its interaction with metallic species is an important tool for understanding the structure of the humic fractions. Fluorescence spectroscopy has been studied as a source of information about what is happening at the molecular level in these compounds. Specially, soils of Amazon region are an important ecosystem of the planet. The aim of this study is to understand the molecular and structural composition of HA samples from Spodosol of Amazonia using the fluorescence Emission-Excitation Matrix (EEM) and Time Resolved Fluorescence Spectroscopy (TRFS). The results showed that the samples of HA showed two fluorescent components; one has a more complex structure and the other one has a simpler structure, which was also seen in TRFS through the evaluation of each sample lifetime. Thus, studies of this nature become important because it aims to evaluate the molecular and structural characteristics of the humic fractions in the region that is considered as one of the most important regions in the world, the Amazon.

Keywords: Amazonian soil, characterization, fluorescence, humic acid, lifetime

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1833 Iron and/or Titanium Containing Microporous Silico-Alumino-Phosphates as a Photocatalyst for Hydrogen Production by Water Splitting

Authors: I. Ben Kaddour, S. Larbaoui

Abstract:

Since their first synthesis, the Silicoaluminophosphates materials have proved their efficiency as a good adsorbent and catalyst in several environmental and energetic applications. In this work, the photocatalytic hydrogen production from water splitting reactions has been conducted under visible radiations in the presence of a series of iron and/or titanium-containing microporous silico-alumino-phosphates materials synthesized by hydrothermal method, using triethylamine as an organic structuring agent to obtain the AFI structure type. These photo-catalysts were then characterized by various physicochemical methods to determine their structural, textural and morphological properties such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) coupled with X rays microanalysis, nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS), and X-rays photoelectron spectroscopy (XPS) and the analysis revealed that these materials have significant photocatalytic properties. The hydrogen production process has been followed by photoelectrochemical characterization (PEC). The results showed that hydrogen is the only gas produced, and the reaction takes place in the conduction band where water is reduced to hydrogen. The electron recombination has also been avoided, as holes are entrapped using hole scavengers. In addition, these catalysts have been shown to remain stable during reuse for up to five cycles.

Keywords: photocatalysis, SAPO-5, hydrothermal synthesis, hydrogen production

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1832 Preparation and Structural Analysis of Nano-Ciprofloxacin by Fourier Transform X-Ray Diffraction, Infra-Red Spectroscopy, and Semi Electron Microscope (SEM)

Authors: Shahriar Ghammamy, Mehrnoosh Saboony

Abstract:

Purpose: To evaluate the spectral specification (IR-XRD and SEM) of nano-ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and its characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation enhances the antibacterial property of nano-ciprofloxacin in comparison to ciprofloxacin. IR spectrum of nano-ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano-ciprofloxacin were sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano-ciprofloxacin shows the diameter of particles equal to 90.9nm. (on the basis of Scherer Equation). SEM image shows the global shape for nano-ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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1831 Preparation and Structural Analysis of Nano Ciprofloxacin by Fourier Transform Infra-Red Spectroscopy, X-Ray Diffraction and Semi Electron Microscope (SEM)

Authors: Shahriar Ghammamy, Mehrnoosh Saboony

Abstract:

Purpose: to evaluate the spectral specification(IR-XRD and SEM) of nano ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and it,s characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation: to enhance the antibacterial property of nano ciprofloxacin in comparison to ciprofloxacin.IR spectrum of nano ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano ciprofloxacin was sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano ciprofloxacin showes the diameter of particles equal to 90.9 nm (on the basis of scherrer equation). SEM image showes the global shape for nano ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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1830 The Development of a Miniaturized Raman Instrument Optimized for the Detection of Biosignatures on Europa

Authors: Aria Vitkova, Hanna Sykulska-Lawrence

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In recent years, Europa has been one of the major focus points in astrobiology due to its high potential of harbouring life in the vast ocean underneath its icy crust. However, the detection of life on Europa faces many challenges due to the harsh environmental conditions and mission constraints. Raman spectroscopy is a highly capable and versatile in-situ characterisation technique that does not require any sample preparation. It has only been used on Earth to date; however, recent advances in optical and laser technology have also allowed it to be considered for extraterrestrial exploration. So far, most efforts have been focused on the exploration of Mars, the most imminent planetary target. However, as an emerging technology with high miniaturization potential, Raman spectroscopy also represents a promising tool for the exploration of Europa. In this study, the capabilities of Raman technology in terms of life detection on Europa are explored and assessed. Spectra of biosignatures identified as high priority molecular targets for life detection on Europa were acquired at various excitation wavelengths and conditions analogous to Europa. The effects of extremely low temperatures and low concentrations in water ice were explored and evaluated in terms of the effectiveness of various configurations of Raman instruments. Based on the findings, a design of a miniaturized Raman instrument optimized for in-situ detection of life on Europa is proposed.

Keywords: astrobiology, biosignatures, Europa, life detection, Raman Spectroscopy

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1829 Selective and Highly Sensitive Measurement of ¹⁵NH₃ Using Photoacoustic Spectroscopy for Environmental Applications

Authors: Emily Awuor, Helga Huszar, Zoltan Bozoki

Abstract:

Isotope analysis has found numerous applications in the environmental science discipline, most common being the tracing of environmental contaminants on both regional and global scales. Many environmental contaminants contain ammonia (NH₃) since it is the most abundant gas in the atmosphere and its largest sources are from agricultural and industrial activities. NH₃ isotopes (¹⁴NH₃ and ¹⁵NH₃) are therefore important and can be used in the traceability studies of these atmospheric pollutants. The goal of the project is the construction of a photoacoustic spectroscopy system that is capable of measuring ¹⁵NH₃ isotope selectively in terms of its concentration. A further objective is for the system to be robust, easy-to-use, and automated. This is provided by using two telecommunication type near-infrared distributed feedback (DFB) diode lasers and a laser coupler as the light source in the photoacoustic measurement system. The central wavelength of the lasers in use was 1532 nm, with the tuning range of ± 1 nm. In this range, strong absorption lines can be found for both ¹⁴NH₃ and ¹⁵NH₃. For the selective measurement of ¹⁵NH₃, wavelengths were chosen where the cross effect of ¹⁴NH₃ and water vapor is negligible. We completed the calibration of the photoacoustic system, and as a result, the lowest detectable concentration was 3.32 ppm (3Ϭ) in the case of ¹⁵NH₃ and 0.44 ppm (3Ϭ) in the case of ¹⁴NH₃. The results are most useful in the environmental pollution measurement and analysis.

Keywords: ammonia isotope, near-infrared DFB diode laser, photoacoustic spectroscopy, environmental monitoring

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1828 Detection of Epinephrine in Chicken Serum at Iron Oxide Screen Print Modified Electrode

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

Abstract:

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

Procedia PDF Downloads 134
1827 Detection and Quantification of Active Pharmaceutical Ingredients as Adulterants in Garcinia cambogia Slimming Preparations Using NIR Spectroscopy Combined with Chemometrics

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

Abstract:

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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1826 Geometrical Fluid Model for Blood Rheology and Pulsatile Flow in Stenosed Arteries

Authors: Karan Kamboj, Vikramjeet Singh, Vinod Kumar

Abstract:

Considering blood to be a non-Newtonian Carreau liquid, this indirect numerical model investigates the pulsatile blood flow in a constricted restricted conduit that has numerous gentle stenosis inside the view of an increasing body speed. Asymptotic answers are obtained for the flow rate, pressure inclination, speed profile, sheer divider pressure, and longitudinal impedance to stream after the use of the twofold irritation approach to the problem of the succeeding non-straight limit esteem. It has been observed that the speed of the blood increases when there is an increase in the point of tightening of the conduit, the body speed increase, and the power regulation file. However, this rheological manner of behaving changes to one of longitudinal impedance to stream and divider sheer pressure when each of the previously mentioned boundaries increases. It has also been seen that the sheer divider pressure in the bloodstream greatly increases when there is an increase in the maximum depth of the stenosis but that it significantly decreases when there is an increase in the pulsatile Reynolds number. This is an interesting phenomenon. The assessments of the amount of growth in the longitudinal resistance to flow increase overall with the increment of the maximum depth of the stenosis and the Weissenberg number. Additionally, it is noted that the average speed of blood increases noticeably with the growth of the point of tightening of the corridor, and body speed increases border. This is something that can be observed.

Keywords: geometry of artery, pulsatile blood flow, numerous stenosis

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1825 White Wine Discrimination Based on Deconvoluted Surface Enhanced Raman Spectroscopy Signals

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

Abstract:

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

Procedia PDF Downloads 131
1824 Magnetron Sputtered Thin-Film Catalysts with Low Noble Metal Content for Proton Exchange Membrane Water Electrolysis

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

Abstract:

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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1823 Synthesis and Characterization of Pure and Doped Li7La3Zr2O12 Li-Ion Conducting Solid Electrolyte for Lithium Batteries

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

Abstract:

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

Procedia PDF Downloads 231
1822 Electrical and Optical Properties of Polyaniline: Cadmium Sulphide Quantum Dots Nanocomposites

Authors: Akhtar Rasool, Tasneem Zahra Rizvi

Abstract:

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

Procedia PDF Downloads 227