Search results for: spectroscopy data analysis

Authors: Ali Moafi, Kourosh Kalantarzadeh, Richard Kaner, Parviz Parvin, Ebrahim Asl Soleimani, Dougal McCulloch

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In-situ Raman spectroscopy of flexible graphene-oxide films examined upon exposure to hydrogen gas, air, and synthetic air. The changes in D and G peaks are attributed to defects responding to atomic hydrogen spilled over from the catalytic behavior of Pt nanoparticles distributed all over the film. High-resolution transmission electron microscopy images (HRTEM) as well as electron energy loss spectroscopy (EELS) were carried out to define the density of the samples.

Keywords: in situ Raman Spectroscopy, EELS, TEM, graphene oxide, graphene, atomic hydrogen

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Authors: V. Sivakumar, R. Neelakantan

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Mineral mapping on the Moon surface provides the clue to understand the origin, evolution, stratigraphy and geological history of the Moon. Recently, reflectance imaging spectroscopy plays a significant role in identifying minerals on the planetary surface in the Visible to NIR region of the electromagnetic spectrum. The Moon Mineralogy Mapper (M3) onboard Chandrayaan-1 provides unprecedented spectral data of lunar surface to study about the Moon surface. Here we used the M3 sensor data (hyperspectral imaging spectroscopy) for analysing mineralogy of Orientale basin region on the Moon surface. Reflectance spectrums were sampled from different locations of the basin and continuum was removed using ENvironment for Visualizing Images (ENVI) software. Reflectance spectra of unknown mineral composition were compared with known Reflectance Experiment Laboratory (RELAB) spectra for discriminating mineralogy. Minerals like olivine, Low-Ca Pyroxene (LCP), High-Ca Pyroxene (HCP) and plagioclase were identified. In addition to these minerals, an unusual type of spectral signature was identified, which indicates the probable Fe-Mg-spinel lithology in the basin region.

Keywords: chandryaan-1, moon mineralogy mapper, mineral, mare orientale, moon

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Authors: Lamia L. G. Al-Mahamad, Benjamin R. Horrocks, Andrew Houlton

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Hydrogels based on metal coordination polymers of nucleosides and a range of metal ions (Au, Ag, Cu) have been prepared and characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and powder X-ray diffraction. AFM images of the xerogels revealed the formation of extremely long polymer molecules (> 10 micrometers, the maximum scan range). This result is also consistent with TEM images which show a fibrous morphology. Oxidative doping of the Au-nucleoside fibres produces an electrically conductive nanowire. No sharp Bragg peaks were found at the at the X-ray diffraction pattern for metal ions hydrogels indicating that the samples were amorphous, but instead the data showed broad peaks in the range 20 < Q < 40 and correspond to distances d=2μ/Q. The data was analysed using a simplified Rietveld method by fitting a regression model to obtain the distance between atoms.

Keywords: hydrogel, metal ions, nanowire, nucleoside

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy (FTIR), micro-Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

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Authors: E. M. AbdelRazek, G. S. ElBahy, M. A. Allam, A. M. Abdelghany, A. M. Hezma

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Polymeric biocomposite of hydroxyapatite/polyacrylic acid were prepared and their thermal and mechanical properties were improved by addition of cellulose acetate. FTIR spectroscopy technique and X-ray diffraction analysis were employed to examine the physical and chemical characteristics of the biocomposites. Scanning electron microscopy shows a uniform distribution of HAp nano-particles through the polymeric matrix of two organic/inorganic composites weight ratios (60/40 and 70/30), at which the material crystallinity reaches a considerable value appropriate for the needed applications were studied and revealed that the HAp nano-particles are uniformly distributed in the polymeric matrix. Kinetic parameters were determined from the weight loss data using non isothermal thermogravimetric analysis (TGA). Also, the main degradation steps were described and discussed. The mechanical properties of composites were evaluated by measuring tensile strength and elastic modulus. The data indicate that the addition of cellulose acetate can make homogeneous composites scaffold significantly resistant to higher stress. Elastic modulus of the composites was also improved by the addition of cellulose acetate, making them more appropriate for bioapplications.

Keywords: biocomposite, chemical synthesis, infrared spectroscopy, mechanical properties

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Authors: Bhargav Baruah, Ali Shemsedin Reshad, Pankaj Tiwari

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This work presents a detailed study on the thermal degradation kinetics of co-pyrolysis of oil shale of Upper Assam, India with rubber seed shell, and lab-scale pyrolysis to investigate the influence of pyrolysis parameters on product yield and composition of products. The physicochemical characteristics of oil shale and rubber seed shell were studied by proximate analysis, elemental analysis, Fourier transform infrared spectroscopy and X-ray diffraction. The physicochemical study showed the mixture to be of low moisture, high ash, siliceous, sour with the presence of aliphatic, aromatic, and phenolic compounds. The thermal decomposition of the oil shale with rubber seed shell was studied using thermogravimetric analysis at heating rates of 5, 10, 20, 30, and 50 °C/min. The kinetic study of the oil shale pyrolysis process was performed on the thermogravimetric (TGA) data using three model-free isoconversional methods viz. Friedman, Flynn Wall Ozawa (FWO), and Kissinger Akahira Sunnose (KAS). The reaction mechanisms were determined using the Criado master plot. The understanding of the composition of Indian oil shale and rubber seed shell and pyrolysis process kinetics can help to establish the experimental parameters for the extraction of valuable products from the mixture. Response surface methodology (RSM) was employed usinf central composite design (CCD) model to setup the lab-scale experiment using TGA data, and optimization of process parameters viz. heating rate, temperature, and particle size. The samples were pre-dried at 115°C for 24 hours prior to pyrolysis. The pyrolysis temperatures were set from 450 to 650 °C, at heating rates of 2 to 20°C/min. The retention time was set between 2 to 8 hours. The optimum oil yield was observed at 5°C/min and 550°C with a retention time of 5 hours. The pyrolytic oil and gas obtained at optimum conditions were subjected to characterization using Fourier transform infrared spectroscopy (FT-IR) gas chromatography and mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR).

Keywords: Indian oil shale, rubber seed shell, co-pyrolysis, isoconversional methods, gas chromatography, nuclear magnetic resonance, Fourier transform infrared spectroscopy

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Authors: Rafiuddin

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Solid polymer electrolytes have emerged as an area of interest in the field of solid state chemistry owing to their facile and cost-effective synthesis and number of applications in different areas of chemistry, extending over a wide range of temperatures. In the present work, polymer composite solid electrolyte comprising of Polyaniline (PANI) as polymer and potassium silver iodide (KAg4I5) using alumina (Al2O3) of different compositions having the formula (1-x) PANI- KAg4I5. x Al2O3 with x ranging from 0.0 to 0.5 was prepared by solid state reaction method. The structural elucidation and characterization was done by X- Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric- Differential Thermal Analysis (TG-DTA) and Impedance Spectroscopy. The thermal analysis shows a phase transition at 147°C attributed to β-α phase transition of AgI due to the disproportionation of KAg4I5 to AgI and KAg2I3 at temperatures higher than 36°C. The X Ray diffraction analysis also confirms the presence of both AgI and KAg2I3 in the samples. The conductivities recorded over a temperature range of 40-250° C lie in the range of 10-1 to 10-3 S cm-1. Maximum conductivity was seen in the compositon x = 0.4 i.e. 1.84 × 10-2 Scm-1 at 313 K and 1.38 × 10-1 Scm-1 at 513 K, with a minimum activation energy of 0.14 eV.

Keywords: polymer solid electrolytes, XRD, DTA, electrical conductivity, impedance spectroscopy

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Authors: Rafay Ahmed, Condon Lau

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Bone healing is a complex and sequential process involving changes at the molecular level. Raman spectroscopy is a promising technique to study bone mineral and matrix environments simultaneously. In this study, subcritical calvarial defects are used to study bone composition during healing without discomposing the fracture. The model allowed to monitor the natural healing of bone avoiding mechanical harm to the callus. Calvarial defects were created using 1mm burr drill in the parietal bones of Sprague-Dawley rats (n=8) that served in vivo defects. After 7 days, their skulls were harvested after euthanizing. One additional defect per sample was created on the opposite parietal bone using same calvarial defect procedure to serve as control defect. Raman spectroscopy (785 nm) was established to investigate bone parameters of three different skull surfaces; in vivo defects, control defects and normal surface. Principal component analysis (PCA) was utilized for the data analysis and interpretation of Raman spectra and helped in the classification of groups. PCA was able to distinguish in vivo defects from normal surface and control defects. PC1 shows that the major variation at 958 cm⁻¹, which corresponds to ʋ1 phosphate mineral band. PC2 shows the major variation at 1448 cm⁻¹ which is the characteristic band of CH2 deformation and corresponds to collagens. Raman parameters, namely, mineral to matrix ratio and crystallinity was found significantly decreased in the in vivo defects compared to surface and controls. Scanning electron microscope and optical microscope images show the formation of newly generated matrix by means of bony bridges of collagens. Optical profiler shows that surface roughness increased by 30% from controls to in vivo defects after 7 days. These results agree with Raman assessment parameters and confirm the new collagen formation during healing.

Keywords: Raman spectroscopy, principal component analysis, calvarial defects, tissue characterization

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Authors: K. Petcharaporn

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The external characteristics of tomatoes, such as freshness, color and size are typically used in quality control processes for tomatoes sorting. However, the internal mold infection of intact tomato cannot be sorted based on a visible assessment and destructive method alone. In this study, a non-destructive technique was used to predict the internal mold infection of intact tomatoes by using transmittance visible and near infrared (VIS-NIR) spectroscopy. Spectra for 200 samples contained 100 samples for normal tomatoes and 100 samples for mold infected tomatoes were acquired in the wavelength range between 665-955 nm. This data was used in conjunction with partial least squares-discriminant analysis (PLS-DA) method to generate a classification model for tomato quality between groups of internal mold infection of intact tomato samples. For this task, the data was split into two groups, 140 samples were used for a training set and 60 samples were used for a test set. The spectra of both normal and internally mold infected tomatoes showed different features in the visible wavelength range. Combined spectral pretreatments of standard normal variate transformation (SNV) and smoothing (Savitzky-Golay) gave the optimal calibration model in training set, 85.0% (63 out of 71 for the normal samples and 56 out of 69 for the internal mold samples). The classification accuracy of the best model on the test set was 91.7% (29 out of 29 for the normal samples and 26 out of 31 for the internal mold tomato samples). The results from this experiment showed that transmittance VIS-NIR spectroscopy can be used as a non-destructive technique to predict the internal mold infection of intact tomatoes.

Keywords: tomato, mold, quality, prediction, transmittance

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Authors: K. Petcharaporn, N. Prathengjit

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The external characteristics of tomatoes, such as freshness, color and size are typically used in quality control processes for tomatoes sorting. However, the internal mold infection of intact tomato cannot be sorted based on a visible assessment and destructive method alone. In this study, a non-destructive technique was used to predict the internal mold infection of intact tomatoes by using transmittance visible and near infrared (VIS-NIR) spectroscopy. Spectra for 200 samples contained 100 samples for normal tomatoes and 100 samples for mold infected tomatoes were acquired in the wavelength range between 665-955 nm. This data was used in conjunction with partial least squares-discriminant analysis (PLS-DA) method to generate a classification model for tomato quality between groups of internal mold infection of intact tomato samples. For this task, the data was split into two groups, 140 samples were used for a training set and 60 samples were used for a test set. The spectra of both normal and internally mold infected tomatoes showed different features in the visible wavelength range. Combined spectral pretreatments of standard normal variate transformation (SNV) and smoothing (Savitzky-Golay) gave the optimal calibration model in training set, 85.0% (63 out of 71 for the normal samples and 56 out of 69 for the internal mold samples). The classification accuracy of the best model on the test set was 91.7% (29 out of 29 for the normal samples and 26 out of 31 for the internal mold tomato samples). The results from this experiment showed that transmittance VIS-NIR spectroscopy can be used as a non-destructive technique to predict the internal mold infection of intact tomatoes.

Keywords: tomato, mold, quality, prediction, transmittance

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Authors: Syahira Ibrahim, Herlina Abdul Rahim

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The amylose content is an essential element in determining the texture and taste of rice grains. This paper evaluates the use of VIS-SWNIRS in estimating the amylose content for seven varieties of rice grains available in the Malaysian market. Each type consists of 30 samples and all the samples are scanned using the spectroscopy to obtain a range of values between 680-1000nm. The Savitzky-Golay (SG) smoothing filter is applied to each sample’s data before the Principal Component Regression (PCR) technique is used to examine the data and produce a single value for each sample. This value is then compared with reference values obtained from the standard iodine colorimetric test in terms of its coefficient of determination, R2. Results show that this technique produced low R2 values of less than 0.50. In order to improve the result, the range should include a wavelength range of 1100-2500nm and the number of samples processed should also be increased.

Keywords: amylose content, diffuse reflectance, Malaysia rice grain, principal component regression (PCR), Visible and Shortwave near-infrared spectroscopy (VIS-SWNIRS)

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Authors: Hanan Alenezi

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Membrane performance depends on the kind of solvent used in preparation. A membrane made by Polyetherimide (PEI) was evaluated for gas separation using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), and Energy Dispersive X-Ray Spectroscopy (EDS). The purity and the thickness are detected to evaluate the membrane in order to optimize PEI membrane preparation.

Keywords: Energy Dispersive X-Ray Spectroscopy (EDS), Membrane, Polyetherimide PEI, Scanning electron microscope (SEM), Solvent, X-Ray Diffraction (XRD)

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Authors: Radka Sefcu, Vaclava Antuskova, Ivana Turkova

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A growing market with modern artworks of a high price leads to the creation and selling of artwork counterfeits. Material analysis is an important part of the process of assessment of authenticity. Knowledge of materials and techniques used by original authors is also necessary. The contribution presents possibilities of non-invasive methods of structural analysis in research on paintings. It was proved that unambiguous identification of many art materials is feasible without sampling. The combination of Raman spectroscopy with FTIR-external reflection enabled the identification of pigments and binders on selected artworks of prominent Czech painters from the first half of the 20th century – Josef Čapek, Emil Filla, Václav Špála and Jan Zrzavý. Raman spectroscopy confirmed the presence of a wide range of white pigments - lead white, zinc white, titanium white, barium white and also Freeman's white as a special white pigment of painting. Good results were obtained for red, blue and most of the yellow areas. Identification of green pigments was often impossible due to strong fluorescence. Oil was confirmed as a binding medium on most of the analyzed artworks via FTIR - external reflection. Collected data present the valuable background for the determination of art materials characteristic for each painter (his palette) and its development over time. Obtained results will further serve as comparative material for the authentication of artworks. This work has been financially supported by the project of the Ministry of the Interior of the Czech Republic: The Development of a Strategic Cluster for Effective Instrumental Technological Methods of Forensic Authentication of Modern Artworks (VJ01010004).

Keywords: non-invasive analysis, Raman spectroscopy, FTIR-external reflection, forgeries

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Authors: Hyery Kang, Dong-Yeun Koh, Yun-Ho Ahn, Huen Lee

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Determination of the behavior of clathrate hydrate with inhibitor in the THz region will provide useful information about hydrate plug control in the upstream of the oil and gas industry. In this study, terahertz time-domain spectroscopy (THz-TDS) revealed the inhibition of the THF clathrate hydrate system with dosage of polyvinylpyrrolidone (PVP) with three different molecular weights. Distinct footprints of phase transition in the THz region (0.4–2.2 THz) were analyzed and absorption coefficients and real part of refractive indices are obtained in the temperature range of 253 K to 288 K. Along with the optical properties, ring breathing and stretching modes for different molecular weights of PVP in THF hydrate are analyzed by Raman spectroscopy.

Keywords: clathrate hydrate, terahertz spectroscopy, tetrahydrofuran, inhibitor

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Authors: Nipin Kohli, Ravi Chand Singh

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Diabetes mellitus is a serious illness and can be life-threatening if left untreated. Acetone present in the exhaled breath of a diabetic person is a biomarker of patients suffering from diabetes mellitus and is higher than its usual concentration present in the breath of healthy people. In the present work, a portable gas sensor system based on chromium oxide (Cr₂O₃) nanoparticles has been developed that can analyze diabetic patient’s breath. Undoped and indium (In) doped Cr₂O₃ nanoparticles were synthesized by a chemical route and characterized by X-ray diffraction, scanning electron microscopy, Raman spectroscopy, UV-visible spectroscopy, and photoluminescence spectroscopy for their structural, morphological and optical properties. Thick film gas sensors were fabricated out of synthesized samples. To diagnose diabetes, the sensors’ response to low concentrations of acetone was measured, and it was found that the addition of indium dramatically enhances the acetone gas sensing response. Moreover, the fabricated sensors were highly stable, reproducible and resistant to humidity. Enhancement of sensor response of doped sensors towards acetone can be ascribed to increase in defects due to addition of a dopant, and it was found that in-doped Cr₂O₃ sensors are more useful for analysis of breath of diabetic patients.

Keywords: Diabetes mellitus, nanoparticles, raman spectroscopy, sensor

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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, and 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, 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: I. Ben Kaddour, S. Larbaoui

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Since their first synthesis in 1984, silicoaluminophosphates have proven their effectiveness as a good adsorbent and catalyst in several environmental and energy applications. In this work, the photocatalytic reaction of the photo-degradation of a pharmaceutical product in water was carried out in the presence of a series of materials based on titanium oxide, anatase phase, supported on the microporous framework of the SAPO4-5 at different levels, under ultraviolet light. These photo-catalysts were characterized by different physicochemical analysis methods in order to determine their structural, textural, and morphological properties, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), microscopy scanning electronics (SEM), nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS). In this study, liquid chromatography coupled with spectroscopy of mass (LC-MS) was used to determine the nature of the intermediate products formed during the photocatalytic degradation of DCF.

Keywords: photocatalysis, titanium dioxide, SAPO-5, diclofenac

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Authors: Bakhtishod Matmuratov, Sakhiba Madraximova, Rakhmat Esanov, Alimjan Matchanov

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Studies have been performed to obtain complexes of glycyrrhizic acid and kinetins in a 2:1 ratio. The complex of glycyrrhizic acid and kinetins in a 2:1 ratio was considered evidence of the formation of a molecular complex by determining the molecular masses using chromato-mass spectroscopy and analyzing the IR spectra.

Keywords: monoammonium salt of glycyrrhizic acid, glycyrrhizic acid, supramolecular complex, isomolar series, IR spectroscopy

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Authors: Sabir Hussain, Mujtaba Hassan, Kashif Rasool, Asif Shahzad

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Fine particulate matter with an aerodynamic diameter of less than 2.5 μm (PM2.5) was collected in Islamabad from November 2022 to January 2023, at urban sites. The average mass concentrations of PM2.5 varied, ranging from 90.5 to 133 μg m−3 in urban areas. Environmental scanning electron microscopy (ESEM) analysis revealed that Islamabad's PM2.5 comprised soot aggregates, ashes, minerals, bio-particles, and unidentified particles. Results from inductively coupled plasma atomic emission spectroscopy (ICP-OES) indicated a gradual increase in total elemental concentrations in Islamabad PM2.5 in winter, with relatively high levels in December. Significantly different elemental compositions were observed in urban PM2.5. Enrichment factor (EF) analysis suggested that elements such as K, Na, Ca, Mg, Al, Fe, Ba, and Sr were of natural origin, while As, Cu, Zn, Pb, Cd, Mn, Ni, and Se originated from anthropogenic sources. Plasmid DNA assays demonstrated varying levels of potential toxicity in Islamabad PM2.5 collected from urban sites, as well as across different seasons. Notably, the urban winter PM2.5 sample exhibited much stronger toxicity compared to other samples. The presence of heavy metals in Islamabad PM2.5, including Cu, Zn, Pb, Cd, Cr, Mn, and Ni, may have synergistic effects on human health.

Keywords: islamabad particulate matter pm2.5, scanning electron microscopy with energy-dispersive x-ray spectroscopy(sem-eds), fourier transform infrared spectroscopy(ftir), inductively coupled plasma optical emission spectroscopy(icp-oes)

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Jaromir Havlica, Lukas Kalina, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

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In this work, CoFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) spinel ferrite nanoparticles are synthesized by sonochemical method. The structural properties and cation distribution are investigated using X-ray Diffraction (XRD), Raman Spectroscopy, Fourier Transform Infrared Spectroscopy and X-ray photoelectron spectroscopy. The morphology and elemental analysis are screened using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. The particle size measured by FE-SEM and XRD analysis confirm the formation of nanoparticles in the range of 7-10 nm. The electrical properties show that the Gd³⁺ doped cobalt ferrite (CoFe₂₋ₓGdₓO₄; x= 0.20) exhibit enhanced dielectric constant (277 at 100 Hz) and ac conductivity (20.17 x 10⁻⁹ S/cm at 100 Hz). The complex impedance measurement study reveals that as Gd³⁺ doping concentration increases, the impedance Z’ and Z’ ’ decreases. The influence of Gd³⁺ doping in cobalt ferrite nanoparticles on the magnetic property is examined by using vibrating sample magnetometer. Magnetic property measurement reveal that the coercivity decreases with Gd³⁺ substitution from 234.32 Oe (x=0.00) to 12.60 Oe (x=0.05) and further increases from 12.60 Oe (x=0.05) to 68.62 Oe (x=0.20). The saturation magnetization decreases with Gd³⁺ substitution from 40.19 emu/g (x=0.00) to 21.58 emu/g (x=0.20). This decrease follows the three-sublattice model suggested by Yafet-Kittel (Y-K). The Y-K angle increases with the increase of Gd³⁺ doping in cobalt ferrite nanoparticles.

Keywords: sonochemical method, nanoparticles, magnetic property, dielectric property, electrical property

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Authors: Disha Gupta

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The aim of this research is to conduct X-ray and e-beam characterization techniques on lithium-ion battery materials for the improvement of battery performance. The key characterization techniques employed are the synchrotron X-ray Absorption Spectroscopy (XAS) combined with X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to obtain a more holistic approach to understanding material properties. This research effort provides additional battery characterization knowledge that promotes the development of new cathodes, anodes, electrolyte and separator materials for batteries, hence, leading to better and more efficient battery performance. Both ex-situ and in-situ synchrotron experiments were performed on LiFePO₄, one of the most common cathode material, from different commercial sources and their structural analysis, were conducted using Athena/Artemis software. This analysis technique was then further extended to study other cathode materials like LiMnxFe(₁₋ₓ)PO₄ and even some sulphate systems like Li₂Mn(SO₄)₂ and Li₂Co0.5Mn₀.₅ (SO₄)₂. XAS data were collected for Fe and P K-edge for LiFePO4, and Fe, Mn and P-K-edge for LiMnxFe(₁₋ₓ)PO₄ to conduct an exhaustive study of the structure. For the sulphate system, Li₂Mn(SO₄)₂, XAS data was collected at both Mn and S K-edge. Finite Difference Method for Near Edge Structure (FDMNES) simulations were also conducted for various iron, manganese and phosphate model compounds and compared with the experimental XANES data to understand mainly the pre-edge structural information of the absorbing atoms. The Fe K-edge XAS results showed a charge compensation occurring on the Fe atom for all the differently synthesized LiFePO₄ materials as well as the LiMnxFe(₁₋ₓ)PO₄ systems. However, the Mn K-edge showed a difference in results as the Mn concentration changed in the materials. For the sulphate-based system Li₂Mn(SO₄)₂, however, no change in the Mn K-edge was observed, even though electrochemical studies showed Mn redox reactions.

Keywords: li-ion batteries, electrochemistry, X-ray absorption spectroscopy, XRD

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Authors: Christine Fräulin, Daniela Schurr, Hamed Shahidi Rad, Gerrit Waters, Günter Rinke, Roland Dittmeyer, Michael Nilles

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The reaction mechanisms of many liquid-phase reactions in organic chemistry have not yet been sufficiently clarified. Process conditions of several hundred degrees celsius and pressures to ten megapascals complicate the sampling and the determination of kinetic data. Space resolved in-situ measurements promises new insights. A non-invasive in-situ measurement technique has the advantages that no sample preparation is necessary, there is no change in sample mixture before analysis and the sampling do no lead to interventions in the flow. Thus, the goal of our research was the development of a contact-free spatially resolved measurement technique for kinetic studies of liquid phase reaction under process conditions. Therefore we used laser Raman spectroscopy combined with an optical transparent microchannel reactor. To show the performance of the system we choose the oxidation of cyclohexane as sample reaction. Cyclohexane oxidation is an economically important process. The products are intermediates for caprolactam and adipic acid, which are starting materials for polyamide 6 and 6.6 production. To maintain high selectivities of 70 to 90 %, the reaction is performed in industry at a low conversion of about six percent. As Raman spectroscopy is usually very selective but not very sensitive the detection of the small product concentration in cyclohexane oxidation is quite challenging. To meet these requirements, an optical experimental setup was optimized to determine the concentrations by laser Raman spectroscopy with respect to good detection sensitivity. With this measurement technique space resolved kinetic studies of uncatalysed and homogeneous catalyzed cyclohexane oxidation were carried out to obtain details about the reaction mechanism.

Keywords: in-situ laser raman spectroscopy, space resolved kinetic measurements, homogeneous catalysis, chemistry

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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: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: A. Guemache, M. Omari

Abstract:

Oxides with formula Ca1-xSrx MnO3 (0≤x≤0.2) were synthesized using co-precipitation method. The identification of the obtained phase was carried out using infrared spectroscopy and X-ray diffraction. Thermogravimetric and differential analysis was permitted to characterize different transformations of precursors which take place during one heating cycle. The study of electrochemical behavior was carried out by cyclic voltammetry and impedance spectroscopy. The obtained results show that apparent catalytic activity improved when increasing the concentration of strontium. Anodic current densities varies from 1.3 to 5.9 mA/cm2 at the rate scan of 20 mV.s-1 and a potential 0.8 V for oxides with composition x=0 to 0.2.

Keywords: oxide, co-precipitation, electrochemical properties, cathode-type

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda

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In this report, the impact of Gd³⁺ substitution in ZnFe₂O₄ spinel ferrite nanoparticles on structural, optical and magnetic properties was investigated. ZnFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) nanoparticles were synthesized by honey-mediated sol-gel combustion method. X-ray diffraction, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy confirmed the formation of cubic spinel ferrite crystal structure. The morphology and elemental analysis were studied using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. UV-Visible reflectance spectroscopy revealed band gap variation with concentration of Gd³⁺ substitution in ZnFe₂O₄ nanoparticles. Magnetic property was studied using vibrating sample magnetometer at room temperature. The synthesized spinel ferrite nanoparticles showed ferromagnetic behaviour. The evaluated magnetic parameters such as saturation magnetization, coercivity and remanence showed variation with Gd³⁺ substitution in spinel ferrite nanoparticles. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: sol-gel combustion method, nanoparticles, magnetic property, optical property

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Authors: Hina Verma, Karine Le Guen, Renaud Dalaunay, Iyas Ismail, Vita Ilakovac, Jean Pascal Rueff, Yunlin Jacques Zheng, Philippe Jonnard

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To the extent of our knowledge, X-ray emission spectroscopy (XES) has been applied in the soft x-ray region (photon energy ≤ 2 keV) to study the buried layers and interfaces of stacks of nanometer-thin films. Now we extend the methodology to study the buried interfaces in the hard X-ray region (i.e., ≥ five keV). The emission spectra allow us to study the interactions between elements in the buried layers from the analysis of their valence states, thereby providing sensitive information about the physical-chemical environment of the emitting element in multilayers. We exploit the chemical sensitivity of XES to study the interfaces between Fe and Si layers in the Fe/Si multilayer from the Fe Kβ₂,₅ emission spectra (7108 eV). The Fe Kβ₅ emission line results from the electronic transition from occupied 3d to 1s levels (i.e., valence to core transition) and is hence sensitive to the chemical state of emitting Fe atoms. The comparison of emission spectra recorded for Fe/Si multilayer with Fe and FeSi₂ references reveal the formation of FeSi₂ at the Fe-Si interfaces inside the multilayer stack. The interfacial thickness was calculated to be 1.4 ± 0.2 nm by taking into consideration the intensity of Fe atoms emitted from the interface and the Fe layer. The formation of FeSi₂ at the interface was further confirmed by the X-ray diffraction and X-ray photoelectron spectroscopy done on the Fe/Si multilayer. Hence, we can conclude that the XES in the hard X-ray range could be used to study multilayers and their interfaces and obtain information both qualitatively and quantitatively.

Keywords: buried interfaces, hard X-ray emission spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy

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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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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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