Search results for: NMR spectroscopy

Authors: Pavel Pořízka, David Prochazka, Karel Novotný, Ota Samek, ZdeněkPilát, Klára Procházková, and Jozef Kaiser

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Themain goal of this article is to find efficient methods for elemental and molecular analysis of living microorganisms (algae) under defined environmental conditions and cultivation processes. The overall knowledge of chemical composition is obtained utilizing laser-based techniques, Laser- Induced Breakdown Spectroscopy (LIBS) for acquiring information about elemental composition and Raman Spectroscopy for gaining molecular information, respectively. Algal cells were suspended in liquid media and characterized using their spectra. Results obtained employing LIBS and Raman Spectroscopy techniques will help to elucidate algae biology (nutrition dynamics depending on cultivation conditions) and to identify algal strains, which have the potential for applications in metal-ion absorption (bioremediation) and biofuel industry. Moreover, bioremediation can be readily combined with production of 3rd generation biofuels. In order to use algae for efficient fuel production, the optimal cultivation parameters have to be determinedleading to high production of oil in selected cellswithout significant inhibition of the photosynthetic activity and the culture growth rate, e.g. it is necessary to distinguish conditions for algal strain containing high amount of higher unsaturated fatty acids. Measurements employing LIBS and Raman Spectroscopy were utilized in order to give information about alga Trachydiscusminutus with emphasis on the amount of the lipid content inside the algal cell and the ability of algae to withdraw nutrients from its environment and bioremediation (elemental composition), respectively. This article can serve as the reference for further efforts in describing complete chemical composition of algal samples employing laserablation techniques.

Keywords: Laser-Induced Breakdown Spectroscopy, Raman Spectroscopy, Algae, Algal strains, Bioremediation, Biofuels.

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Authors: Sie-Tiong Ha, Teck-Leong Lee, Yip-Foo Win, Siew-Ling Lee, Guan-Yeow Yeap

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A homologous series of aromatic esters, 4-nalkanoyloxybenzylidene- 4--bromoanilines, nABBA, consisting of two 1,4-disubstituted phenyl cores and a Schiff base central linkage was synthesized. All the members can be differed by the number of carbon atoms at terminal alkanoyloxy chain (CnH2n-1COO-, n = 2, 6, 18). The molecular structure of nABBA was confirmed with infrared spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and electron-ionization mass (EI-MS) spectrometry. Mesomorphic properties were studied using differential scanning calorimetry and polarizing optical microscopy.

Keywords: Liquid Crystals, Schiff base, Smectic, Mesomorphic

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Authors: Y. El Kaissi, M. Allam, A. Koulou, M. Galai, M. Ebn Touhami

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The aim of our work is to develop an industrial bath of nickel alloy deposit on mild steel. The optimization of the operating parameters made it possible to obtain a stable Ni-P alloy deposition formulation. To understand the reaction mechanism of the deposition process, a kinetic study was performed by cyclic voltammetry and by electrochemical impedance spectroscopy (EIS). The coatings obtained have a very high corrosion resistance in a very aggressive acid medium which increases with the heat treatment.

Keywords: Ni–P coating, electrochemical impedance spectroscopy, heat treatment, cyclic voltammetry, potentiodynamic polarization.

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Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X-ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: Calibration model, celitement, cementitious material, NIR spectroscopy.

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Authors: Khamael M. Abualnaja, Lidija Šiller, Benjamin R. Horrocks

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Alkylated silicon nanocrystals (C11-SiNCs) were prepared successfully by galvanostatic etching of p-Si(100) wafers followed by a thermal hydrosilation reaction of 1-undecene in refluxing toluene in order to extract C11-SiNCs from porous silicon. Erbium trichloride was added to alkylated SiNCs using a simple mixing chemical route. To the best of our knowledge, this is the first investigation on mixing SiNCs with erbium ions (III) by this chemical method. The chemical characterization of C11-SiNCs and their mixtures with Er3+(Er/C11-SiNCs) were carried out using X-ray photoemission spectroscopy (XPS). The optical properties of C11- SiNCs and their mixtures with Er3+ were investigated using Raman spectroscopy and photoluminescence (PL). The erbium mixed alkylated SiNCs shows an orange PL emission peak at around 595 nm that originates from radiative recombination of Si. Er/C11-SiNCs mixture also exhibits a weak PL emission peak at 1536 nm that originates from the intra-4f transition in erbium ions (Er3+). The PL peak of Si in Er/C11-SiNCs mixture is increased in the intensity up to three times as compared to pure C11-SiNCs. The collected data suggest that this chemical mixing route leads instead to a transfer of energy from erbium ions to alkylated SiNCs.

Keywords: Photoluminescence, Silicon Nanocrystals, Erbium, Raman Spectroscopy.

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Authors: M.E.khosroshahi , M.S.Nourbakhsh

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Wet chemistry methods are used to prepare the SiO2/Au nanoshells. The purpose of this research was to synthesize gold coated SiO2 nanoshells for biomedical applications. Tunable nanoshells were prepared by using different colloidal concentrations. The nanoshells are characterized by FTIR, XRD, UV-Vis spectroscopy and atomic force microscopy (AFM). The FTIR results confirmed the functionalization of the surfaces of silica nanoparticles with NH2 terminal groups. A tunable absorption was observed between 470-600 nm with a maximum range of 530-560 nm. Based on the XRD results three main peaks of Au (111), (200) and (220) were identified. Also AFM results showed that the silica core diameter was about 100 nm and the thickness of gold shell about 10 nm.

Keywords: Gold nanoshells, Synthesis, UV-vis spectroscopy, XRD, AFM

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Authors: Maribel G. Guzmán, Jean Dille, Stephan Godet

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Silver nanoparticles were prepared by chemical reduction method. Silver nitrate was taken as the metal precursor and hydrazine hydrate as a reducing agent. The formation of the silver nanoparticles was monitored using UV-Vis absorption spectroscopy. The UV-Vis spectroscopy revealed the formation of silver nanopart├¡cles by exhibing the typical surface plasmon absorption maxima at 418-420 nm from the UV–Vis spectrum. Comparison of theoretical (Mie light scattering theory) and experimental results showed that diameter of silver nanoparticles in colloidal solution is about 60 nm. We have used energy-dispersive spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and, UV–Vis spectroscopy to characterize the nanoparticles obtained. The energy-dispersive spectroscopy (EDX) of the nanoparticles dispersion confirmed the presence of elemental silver signal no peaks of other impurity were detected. The average size and morphology of silver nanoparticles were determined by transmission electron microscopy (TEM). TEM photographs indicate that the nanopowders consist of well dispersed agglomerates of grains with a narrow size distribution (40 and 60 nm), whereas the radius of the individual particles are between 10 and 20 nm. The synthesized nanoparticles have been structurally characterized by X-ray diffraction and transmission high-energy electron diffraction (HEED). The peaks in the XRD pattern are in good agreement with the standard values of the face-centered-cubic form of metallic silver (ICCD-JCPDS card no. 4-0787) and no peaks of other impurity crystalline phases were detected. Additionally, the antibacterial activity of the nanopart├¡culas dispersion was measured by Kirby-Bauer method. The nanoparticles of silver showed high antimicrobial and bactericidal activity against gram positive bacteria such as Escherichia Coli, Pseudimonas aureginosa and staphylococcus aureus which is a highly methicillin resistant strain.

Keywords: Silver nanoparticles, surface plasmon, UV-Vis absorption spectrum, chemicals reduction.

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Authors: Maria V. Morozova, Zoya A. Mikhaylovskaya, Elena S. Buyanova, Sofia A. Petrova, Ksenia V. Arishina, Robert G. Zaharov

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The present work is devoted to the investigation of two series of doped bismuth molybdates: Bi_26-2xMn_2xMo₁₀O_69-d and Bi₂₆Mo_10-2yMn_2yO_69-d. Complex oxides were synthesized by conventional solid state technology and by co-precipitation method. The products were identified by powder diffraction. The powders and ceramic samples were examined by means of densitometry, laser diffraction, and electron microscopic methods. Porosity of the ceramic materials was estimated using the hydrostatic method. The electrical conductivity measurements were carried out using impedance spectroscopy method.

Keywords: Bismuth molybdate, columnar structures, impedance spectroscopy, oxygen ionic conductors.

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Authors: Mandana Amiri, Sima Nouhi, Yashar Azizan-Kalandaragh

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Silver nanostructures have been successfully fabricated by using electrodeposition method onto indium-tin-oxide (ITO) substrate. Scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and ultraviolet-visible spectroscopy (UV-Vis) techniques were employed for characterization of silver nanostructures. The results show nanostructures with different morphology and electrochemical properties can be obtained by various the deposition potentials and times. Electrochemical behavior of the nanostructures has been studied by using cyclic voltammetry. Silver nanostructures exhibits good electrocatalytic activity towards the reduction of H₂O₂. The presented electrode can be employed as sensing element for hydrogen peroxide.

Keywords: Electrochemical sensor, electrodeposition, hydrogen peroxide, silver nanostructures.

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Authors: Uma Thanganathan

Abstract:

The hybrid membranes containing inorganic materials in polymer matrix are identified as a remarkable family of proton conducting hybrid electrolytes. In this work, the proton conducting inorganic/organic hybrid membranes for proton exchange membrane fuel cells (PEMFCs) were prepared using polyvinyl alcohol (PVA), tetraethoxyorthosilane (TEOS) and heteropolyacid (HPA). The synthesized hybrid membranes were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction spectroscopy (XRD), Scanning electron microscopy (SEM) and Thermogravimetry analysis (TGA). The effects of heteropolyacid incorporation on membrane properties, including morphology and thermal stability were extensively investigated.

Keywords: PEMFC, Hybrid membrane, FTIR, TGA, Phosphomolybdic acid

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Authors: C. I. L. Justino, A. C. Freitas, T. A. P. Rocha-Santos, A. C. Duarte

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This work relates the development of an optical fiber (OF) sensor for the detection and quantification of single walled carbon nanotubes in aqueous solutions. The developed OF displays a compact design, it requires less expensive materials and equipment as well as low volume of sample (0.2 mL). This methodology was also validated by the comparison of its analytical performance with that of a standard methodology based on ultraviolet-visible spectroscopy. The developed OF sensor follows the general SDS calibration proposed for OF sensors as a more suitable calibration fitting compared with classical calibrations.

Keywords: Optical fiber sensor, single-walled carbon nanotubes, SDS calibration model, UV-Vis spectroscopy

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Authors: N. Hammouda, K. Belmokre

Abstract:

Paints are the most widely used methods of protection against atmospheric corrosion of metals. The aim of this work was to determine the protective performance of epoxy coating against sea water before and after damage. Investigations are conducted using stationary and non-stationary electrochemical tools such as electrochemical impedance spectroscopy has allowed us to characterize the protective qualities of these films. The application of the EIS on our damaged in-situ painting shows the existence of several capacitive loops which is an indicator of the failure of our tested paint. Microscopic analysis (micrograph) helped bring essential elements in understanding the degradation of our paint condition and immersion training corrosion products.

Keywords: Epoxy Paints, Electrochemical Impedance Spectroscopy, Corrosion Mechanisms, sea water.

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

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One- and two-dimensional carbon nanostructures with sp2 hybridization of carbon atoms (single walled carbon nanotubes 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 nanotubes 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 nanostructures induced by a strong magnetic field.

Keywords: Carbon nanostructures, magnetic field, Raman spectroscopy.

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Authors: Tze Sian Pui, Tushar Bansal, Patthara Kongsuphol, Sunil K. Arya

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We present a label-free biosensor based on electrochemical impedance spectroscopy for the detection of proinflammatory cytokine Tumor Necrosis Factor (TNF-α). Secretion of TNF-α has been correlated to the onset of various diseases including rheumatoid arthritis, Crohn-s disease etc. Gold electrodes were patterned on a silicon substrate and self assembled monolayer of dithiobis-succinimidyl propionate was used to develop the biosensor which achieved a detection limit of ~57fM. A linear relationship was also observed between increasing TNF-α concentrations and chargetransfer resistance within a dynamic range of 1pg/ml – 1ng/ml.

Keywords: Tumor necrosis factor, electrochemical impedance spectroscopy, label free, self assembled monolayer

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Authors: Dije Dehari, Ahmed Jashari, Shefket Dehari, Agim Shabani

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New complexes of nickel (II) have been synthesized in the reaction mixture of nickel (II) acetate and 4-hydroxy-2-oxo-2H-chromene-3-carboxamide. Bis(4-hydroxy-2-oxo-2H-chromene-3-carboxamidato-O,O)nickel (II) and diaquabis(4-hydroxy-2-oxo-2H-chromene-3-carboxamidato-O,O)nickel (II) were characterized by elemental analysis, IR spectroscopy and ESI mass spectrometry. Elemental analysis and mass spectrometry data of the complexes suggests the stoichiometry of 1:2 (metal-ligand).

Keywords: Nickel complexes, 4-hydroxy-2-oxo-2H-chromene-3-carboxamide, IR spectroscopy, mass spectrometry.

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Authors: Haleh Rezaei Zanjirabadi, Fatemeh Saberi, Bahman Rahimzadeh, Fariborz Masoudi, Mohammad Rahgosha

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In this study, apatite minerals from the iron-phosphate deposit of Yazd have been investigated within the microcontinent zone of Iran in the Zagros structural zone. The geological units in the Esfordi area belong to the pre-Cambrian to lower-Cambrian age, consisting of a succession of carbonate rocks (dolomite), shale, tuff, sandstone, and volcanic rocks. In addition to the mentioned sedimentary and volcanic rocks, the granitoid mass of Bahabad, which is the largest intrusive mass in the region, has intruded into the eastern part of this series and has caused its metamorphism and alteration. After collecting the available data, various samples of Esfordi’s apatite were prepared, and their mineralogy and crystallography were investigated using laboratory methods such as petrographic microscopy, Raman spectroscopy, EDS (Energy Dispersive Spectroscopy), and Scanning Electron Microscopy (SEM). In non-destructive Raman spectroscopy, the molecular structure of apatite minerals was revealed in four distinct spectral ranges. Initially, the spectra of phosphate and aluminum bonds with O2HO, OH, were observed, followed by the identification of Cl, OH, Al, Na, Ca and hydroxyl units depending on the type of apatite mineral family. In SEM analysis, based on various shapes and different phases of apatites, their constituent major elements were identified through EDS, indicating that the samples from the Esfordi mining area exhibit a dense and coherent texture with smooth surfaces. Based on the elemental analysis results by EDS, the apatites in the Esfordi area are classified into the calcic apatite group.

Keywords: Petrology, apatite, Esfordi, EDS, SEM, Scanning Electron Microscopy, Raman spectroscopy.

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

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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 multicomponent 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, multicomponent solutions, Raman spectroscopy.

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Authors: Cherry Dhiman, Ayushi Paliwal, Mohd. Shahid Khan, M. N. Reddy, Vinay Gupta, Monika Tomar

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The laser based high resolution spectroscopic experimental techniques such as Laser Induced Breakdown Spectroscopy (LIBS), Rotating Disk Electrode Optical Emission spectroscopy (RDE-OES) and Surface Plasmon Resonance (SPR) have been used for the study of composition and degradation analysis of used engine oils. Engine oils are mainly composed of aliphatic and aromatics compounds and its soot contains hazardous components in the form of fine, coarse and ultrafine particles consisting of wear metal elements. Such coarse particulates matter (PM) and toxic elements are extremely dangerous for human health that can cause respiratory and genetic disorder in humans. The combustible soot from thermal power plants, industry, aircrafts, ships and vehicles can lead to the environmental and climate destabilization. It contributes towards global pollution for land, water, air and global warming for environment. The detection of such toxicants in the form of elemental analysis is a very serious issue for the waste material management of various organic, inorganic hydrocarbons and radioactive waste elements. In view of such important points, the current study on used engine oils was performed. The fundamental characterization of engine oils was conducted by measuring water content and kinematic viscosity test that proves the crude analysis of the degradation of used engine oils samples. The microscopic quantitative and qualitative analysis was presented by RDE-OES technique which confirms the presence of elemental impurities of Pb, Al, Cu, Si, Fe, Cr, Na and Ba lines for used waste engine oil samples in few ppm. The presence of such elemental impurities was confirmed by LIBS spectral analysis at various transition levels of atomic line. The recorded transition line of Pb confirms the maximum degradation which was found in used engine oil sample no. 3 and 4. Apart from the basic tests, the calculations for dielectric constants and refractive index of the engine oils were performed via SPR analysis.

Keywords: Laser induced breakdown spectroscopy, rotating disk electrode optical emission spectroscopy, surface plasmon resonance, ICCD spectrometer, Nd:YAG laser, engine oil.

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Authors: M. Bodner, M. Scampicchio

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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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Authors: Amir Tosson, Mohammad Reza, Christian Gutt

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Metadata is one of the most important aspects for advancing data management practices within all research communities. Definitions and schemes of metadata are inter alia of particular significance in the domain of neutron and photon scattering experiments covering a broad area of different scientific disciplines. The demand of describing continuously evolving highly non-standardized experiments, including the resulting processed and published data, constitutes a considerable challenge for a static definition of metadata. Here, we present the concept of dynamic metadata for the neutron and photon scientific community, which enriches a static set of defined basic metadata. We explore the idea of dynamic metadata with the help of the use case of X-ray Photon Correlation Spectroscopy (XPCS), which is a synchrotron-based scattering technique that allows the investigation of nanoscale dynamic processes. It serves here as a demonstrator of how dynamic metadata can improve data acquisition, sharing, and analysis workflows. Our approach enables researchers to tailor metadata definitions dynamically and adapt them to the evolving demands of describing data and results from a diverse set of experiments. We demonstrate that dynamic metadata standards yield advantages that enhance data reproducibility, interoperability, and the dissemination of knowledge.

Keywords: Big data, metadata, schemas, XPCS, X-ray Photon Correlation Spectroscopy.

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Authors: Prakash Chand, Anurag Gaur, Ashavani Kumar

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In the present study, we have synthesized Cr and Fe doped zinc oxide (ZnO) nanostructures (Zn1-δCraFebO; where δ = a + b = 20%, a = 5, 6, 8 & 10% and b = 15, 14, 12 & 10%) via sol-gel method at different doping concentrations. The synthesized samples were characterized for structural properties by X-ray diffractrometer and field emission scanning electron microscope and the optical properties were carried out through photoluminescence and UVvisible spectroscopy. The particle size calculated through field emission scanning electron microscope varies from 41 to 96 nm for the samples synthesized at different doping concentrations. The optical band gaps calculated through UV-visible spectroscopy are found to be decreasing from 3.27 to 3.02 eV as the doping concentration of Cr increases and Fe decreases.

Keywords: Nanostructures, Optical Properties, Sol-gel method.

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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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Authors: Chen-Fu Wang, Lin-Ya Kung

Abstract:

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: Jana P. Vejpravova, Daniel Niznansky, Vaclav Vales, Barbara Bittova, Vaclav Tyrpekl, Stanislav Danis, Vaclav Holy, Stephen Doyle

Abstract:

The aim of our work is to study phase composition, particle size and magnetic response of Fe2O3/TiO2 nanocomposites with respect to the final annealing temperature. Those nanomaterials are considered as smart catalysts, separable from a liquid/gaseous phase by applied magnetic field. The starting product was obtained by an ecologically acceptable route, based on heterogeneous precipitation of the TiO2 on modified g-Fe2O3 nanocrystals dispersed in water. The precursor was subsequently annealed on air at temperatures ranging from 200 oC to 900 oC. The samples were investigated by synchrotron X-ray powder diffraction (S-PXRD), magnetic measurements and Mössbauer spectroscopy. As evidenced by S-PXRD and Mössbauer spectroscopy, increasing the annealing temperature causes evolution of the phase composition from anatase/maghemite to rutile/hematite, finally above 700 oC the pseudobrookite (Fe2TiO5) also forms. The apparent particle size of the various Fe2O3/TiO2 phases has been determined from the highquality S-PXRD data by using two different approaches: the Rietveld refinement and the Debye method. Magnetic response of the samples is discussed in considering the phase composition and the particle size.

Keywords: X-ray diffraction, profile analysis, Mössbauer spectroscopy, magnetic properties, TiO2, Fe2O3, Fe2TiO5

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

Abstract:

Magnesium wastes and scraps, one of the metal wastes, are produced by many industrial activities, all over the world. Their growing size is becoming a future problem for the world. In this study, the use of magnesium wastes as a raw material in the production of the magnesium borate hydrates are aimed. The method used in the experiments is hydrothermal synthesis. The conditions are set to, waste magnesium to B2O3, 1:3 as a molar ratio. Four different reaction times are studied which are 30, 60, 120 and 240 minutes. For the identification analyses X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman spectroscopy techniques are used. As a result at all the reaction times magnesium borate hydrates are synthesized and the most crystalline forms are obtained at a reaction time of 120 minutes. The overall yields of the production are found between the values of 65-80 %.

Keywords: Hydrothermal synthesis, magnesium borates, magnesium wastes, boron oxide

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Authors: Yongkui Cui, Fengping Wang, Hailai Zhao, Muhammad Zubair Iqbal, Ziya Wang, Yan Li, Pengpeng L. V.

Abstract:

The novel 3D SnO cabbages self-assembled by nanosheets were successfully synthesized via template-free hydrothermal growth method under facile conditions. The XRD results manifest that the as-prepared SnO is tetragonal phase. The TEM and HRTEM results show that the cabbage nanosheets are polycrystalline structure consisted of considerable single-crystalline nanoparticles. Two typical Raman modes A1g=210 and Eg=112 cm-1 of SnO are observed by Raman spectroscopy. Moreover, galvanostatic cycling tests has been performed using the SnO cabbages as anode material of lithium ion battery and the electrochemical results suggest that the synthesized SnO cabbage structures are a promising anode material for lithium ion batteries.

Keywords: Hydrothermal process, lithium ion battery, Raman spectroscopy, stannous oxide.

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

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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.

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Authors: Babajide O. Ogungbesan, Rajneesh Kumar, Mohamed Sassi

Abstract:

Hydrogen sulfide (H2S) is a very toxic gas that is produced in very large quantities in the oil and gas industry. It cannot be flared to the atmosphere and Claus process based gas plants are used to recover the sulfur and convert the hydrogen to water. In this paper, we present optical characterization of an atmospheric pressure microwave plasma torch for H2S dissociation into hydrogen and sulfur. The torch is operated at 2.45 GHz with power up to 2 kW. Three different gases can simultaneously be injected in the plasma torch. Visual imaging and optical emission spectroscopy are used to characterize the plasma for varying gas flow rates and microwave power. The plasma length, emission spectra and temperature are presented. The obtained experimental results validate our earlier published simulation results of plasma torch.

Keywords: Atmospheric pressure microwave plasma, gas dissociation, optical emission spectroscopy.

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Authors: Mohammadhosein Rahimi, Mohammad Raouf Hosseini, Mehran Bakhshi, Alireza Baghbanan

Abstract:

Silver ions (Ag⁺) and their compounds are consequentially toxic to microorganisms, showing biocidal effects on many species of bacteria. Silver-phosphate (or silver orthophosphate) is one of these compounds, which is famous for its antimicrobial effect and catalysis application. In the present study, a green method was presented to synthesis silver-phosphate nanoparticles using Sporosarcina pasteurii. The composition of the biosynthesized nanoparticles was identified as Ag₃PO₄ using X-ray Diffraction (XRD) and Energy Dispersive Spectroscopy (EDS). Also, Fourier Transform Infrared (FTIR) spectroscopy showed that Ag₃PO₄ nanoparticles was synthesized in the presence of biosurfactants, enzymes, and proteins. In addition, UV-Vis adsorption of the produced colloidal suspension approved the results of XRD and FTIR analyses. Finally, Transmission Electron Microscope (TEM) images indicated that the size of the nanoparticles was about 20 nm.

Keywords: Bacteria, biosynthesis, silver-phosphate, Sporosarcina pasteurii, nanoparticle.

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Authors: Marzieh Moosavi-Nasab, Ali R. Yousefi, Hamed Askari, Maryam Bakhtiyari

Abstract:

In this study, static batch fermentation was used for bacterial cellulose production in date syrup solution (Bx. 10%) at 28°C using Gluconacetobacter. xylinus (PTCC 1734). The physicochemical properties of standard Sigma CMC and the produced carboxymethyl bacterial cellulose (CMBC) were studied using FT-IR spectroscopy, X-ray diffractometry (XRD) and Scanning Electron Microscopy (SEM). According to the FT-IR spectra the bands at 1664 and 1431 cm-1 indicate that carboxylic acid groups and carboxylate groups exist on the surface. The SEM imaging of CMBC and CMC carried out in magnification of 1K. Comparing the SEM imaging obviously showed that the ribbon shape in CMC remained but the length of ribbons became shorter while that shape changed to flake shape for CMBC. Determination of the area under XRD patterns demonstrated that the crystallinity amount of CMC was more than that for CMBC (51.08% and 81.84% for CMBC and CMC, respectively).

Keywords: Carboxymethyl bacterial cellulose, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, X-ray diffractometry.

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