Search results for: ftir/raman spectra

Authors: P. Vit, J. Uddin, V. Zuccato, F. Maza, E. Schievano

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In Ecuador honeys are produced by Apis mellifera and stingless bees (Meliponini). We studied honey produced in beeswax combs by Apis mellifera, and honey produced in pots by Geotrigona and Scaptotrigona bees. Chloroform extracts of honey were obtained for fast NMR spectra. The 1D spectra were acquired at 298 K, with a 600 MHz NMR Bruker instrument, using a modified double pulsed field gradient spin echoes (DPFGSE) sequence. Signals of 1H NMR spectra were integrated and used as inputs for PCA, PLS-DA analysis, and labelled sets of classes were successfully identified, enhancing the separation between the three groups of honey according to the entomological origin: A. mellifera, Geotrigona and Scaptotrigona. This procedure is therefore recommended for authenticity test of honey in Ecuador.

Keywords: Apis mellifera, honey, 1H NMR, entomological origin, meliponini

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Authors: Ahmed A. Sedik, Doaa Mahmoud Shuaib

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Brain injury is a cause of disability and death worldwide. Potassium dichromate (PD) is an environmental contaminant widely recognized as teratogenic, carcinogenic, and mutagenic towards animals and humans. The aim of the present study was to investigate the possible neuroprotective effects of tangeretin (TNG) on PD-induced brain injury in rats. Forty male adult Wistar rats were randomly and blindly allocated into four groups (8 rats /group). The first group received saline intranasally (i.n.). The second group received a single dose of PD (2 mg/kg, i.n.). The third group received TNG (50 mg/kg; orally) for 14 days, followed by i.n. of PD on the last day of the experiment. Four groups received TNG (100 mg/kg; orally) for 14 days, followed by i.n. of PD on the last day of the experiment. 18- hours after the final treatment, behavioral parameters, neuro-biochemical indices, FTIR analysis, and histopathological studies were evaluated. Results of the present study revealed that rats intoxicated with PD promoted oxidative stress and inflammation via an increase in MDA and a decrease in Nrf2 signaling pathway and GSH levels with an increase in brain contents of TNF-α, IL-10, and NF-kβ and reduced AKT levels in brain homogenates. Treatment with TNG (100 mg/kg; orally) ameliorated behavioral, cholinergic activities and oxidative stress, decreased the elevated levels of pro-inflammatory mediators; TNF-α, IL-10, and NF-κβ elevated AKT pathway with corrected FTIR spectra with a decrease in brain content of chromium residues detected by atomic absorption spectrometry. Also, TNG administration restored the morphological changes as degenerated neurons and necrosis associated with PD intoxication. Additionally, TNG decreased Caspase-3 expression in the brain of PD rats. TNG plays a crucial role in AKT/Nrf2 pathway that is responsible for their antioxidant, anti-inflammatory effects, and apoptotic pathway against PD-induced brain injury in rats.

Keywords: tangeretin, potassium dichromate, brain injury, AKT/Nrf2 signaling pathway, FTIR, atomic absorption spectrometry

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Authors: A. Almohammedi, A. J. Hudson, N. M. Storey

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Following ischaemia/reperfusion injury, as in a myocardial infraction, cardiac myocytes undergo oxidative stress which leads to several potential outcomes including; necrotic or apoptotic cell death or dysregulated calcium homeostasis or disruption of the electron transport chain. Several studies have shown that nitric oxide donors protect cardiomyocytes against ischemia and reperfusion. However until present, the mechanism of cardioprotective effect of nitric oxide donor in isolated ventricular cardiomyocytes is not fully understood and has not been investigated before using Raman spectroscopy. For these reasons, the aim of this study was to develop a novel technique, pre-resonance Raman spectroscopy, to investigate the mechanism of cardioprotective effect of nitric oxide donor in isolated ventricular cardiomyocytes exposed to metabolic inhibition and re-energisation. The results demonstrated the first time that Raman microspectroscopy technique has the capability to monitor the metabolic inhibition of cardiomyocytes and to monitor the effectiveness of cardioprotection by nitric oxide donor prior to metabolic inhibition of cardiomyocytes. Metabolic inhibition and reenergisation were used in this study to mimic the low and high oxygen levels experienced by cells during ischaemic and reperfusion treatments. A laser wavelength of 488 nm used in this study has been found to provide the most sensitive means of observe the cellular mechanisms of myoglobin during nitric oxide donor preconditioning, metabolic inhibition and re-energisation and did not cause any damage to the cells. The data also highlight the considerably different cellular responses to metabolic inhibition to ischaemia. Moreover, the data has been shown the relationship between the release of myoglobin and chemical ischemia where that the release of myoglobin from the cell only occurred if a cell did not recover contractility.

Keywords: ex vivo biospectroscopy, Raman spectroscopy, biophotonics, cardiomyocytes, ischaemia / reperfusion injury, cardioprotection, nitric oxide donor

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Authors: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

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Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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Authors: Abdullah Al-Nassri, Ahmed Al-Alawi

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Seaweeds are classified into three groups: red, green, and brown. Each group of seaweeds consists of several types that have differences in composition. Even at the species level, there are differences in some ingredients, although in general composition, they are the same. Environmental conditions, availability of nutrients, and maturity stage are the main reasons for composition differences. In this study, two red seaweed species, Melanothamnus somalensis & Gelidium omanense, were collected in September 2021 from Sadh (Dhofar governorate, Oman). Five organic solvents were used sequentially to achieve extraction. The solvents were applied in the following order: hexane, dichloromethane, ethyl acetate, acetone, and methanol. Preparative HPLC (PrepLC) was performed to fraction the extracts. The chemical composition was measured; also, total phenols, flavonoids, and tannins were investigated. The structure of the extracts was analyzed by Fourier-transform infrared spectroscopy (FTIR). Seaweeds demonstrated high differences in terms of chemical composition, total phenolic content (TPC), total flavonoid content (TFC), and total tannin content (TTC). Gelidium omanense showed high moisture content, lipid content and carbohydrates (9.8 ± 0.15 %, 2.29 ± 0.09 % and 70.15 ± 0.42 %, respectively) compared to Melanothamnus somalensis (6.85 ± 0.01 %, 2.05 ± 0.12 % and 52.7 ± 0.36 % respectively). However, Melanothamnus somalensis showed high ash content and protein (27.68 ± 0.40 % and 52.7 ± 0.36 % respectively) compared to Gelidium omanense (8.07 ± 0.39 % and 9.70 ± 0.22 % respectively). Melanothamnus somalensis showed higher elements and minerals content, especially sodium and potassium. This is attributed to the jelly-like structure of Melanothamnus somalensis, which allows storage of more solutes compared to the leafy-like structure of Gelidium omanense. Furthermore, Melanothamnus somalensis had higher TPC in all fractions except the hexane fraction than Gelidium omanense. Except with hexane, TFC in the other solvents’ extracts was significantly different between Gelidium omanense and Melanothamnus somalensis. In all fractions, except dichloromethane and ethyl acetate fractions, there were no significant differences in TTC between Gelidium omanense and Melanothamnus somalensis. FTIR spectra showed variation between fractions, which is an indication of different functional groups.

Keywords: chemical composition, organic extract, Omani seaweeds, biological activity, FTIR

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Authors: Rajesh Kumar Meena, Suman Jhajharia, Goutam Chakraborty

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Plasmonic silver nanoparticles (Ag NPs) was synthesized by chemical reduction method using Trachyspermum Ammi (TA, Ajwain) seeds extract in aqueous medium and AgNO3 solution at different time interval. Reaction time, and concentration of AgNO3 and TA could accelerate the reduction rate of Ag+ and affect AgNPs size and concentration of NPs. Surface plasmon resonance band centered at 420-430 nm (88.78nm) was recognised as first exitonic peak of UV-Vis absorption spectra of AgNPs that used to calculate the particle size (10-30 nm). FTIR results TA supported AgNPs showed decrease in intensity of peaks at 3394, 1716 and 1618 cm-1 with respect to the plain TA indicating the involvement of O-H, carbonyl group and C=C stretching in formation of TA-AgNPs aggregates. The C-O-C and C-N stretching suggested the presence of many phytochemicals on the surface of the NPs. Impedance study reveals that at low concentration of TA the rate of charge transfer is in TA-AgNPs aggregates, found higher than the higher TA concentration condition that confirms the stability of AgNPs in water. Extract reduce silver ions into silver nanoparticles (NPs) of size 6-50nm. Pronounce effect of the time on Ag NPs concentration and particle size, was exhibited by the system These biogenic Ag NPs are characterized using UV- Vis spectrophotometry (UV-Visible), Fourier transformation infrared (FTIR) and XRD. These studies give us inside view of the most probable mechanism of biosynthesis and optoelectronic properties of the as synthesised Ag NPs.

Keywords: antimicrobial activity, bioreduction, capping agent, silver nanoparticles

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Authors: V. V. Srinivasu, Jayashree Das

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Owing to the industrial and technological importance, transition metal (TM) doped ZnO has been widely chosen for many practical applications in electronics and optoelectronics. Besides, though still a controversial issue, the reported room temperature ferromagnetism in transition metal doped ZnO has added a feather to its excellence and importance in current semiconductor research for prospective application in Spintronics. Anticipating non controversial and improved optical and magnetic properties, we adopted co doping method to synthesise polycrystalline Mn:TM (Fe,Ni) and Mn:RE(Gd,Sm) co doped ZnO samples by solid state sintering route with compositions Zn1-x (Mn:Fe/Ni)xO and Zn1-x(Mn:Gd/Sm)xO and sintered at two different temperatures. The structure, composition and optical changes induced in ZnO due to co doping and sintering were investigated by XRD, FTIR, UV, PL and ESR studies. X-ray peak profile analysis (XPPA) and Williamson-Hall analysis carried out shows changes in the values of stress, strain, FWHM and the crystallite size in both the co doped systems. FTIR spectra also show the effect of both type of co doping on the stretching and bending bonds of ZnO compound. UV-Vis study demonstrates changes in the absorption band edge as well as the significant change in the optical band gap due to exchange interactions inside the system after co doping. PL studies reveal effect of co doping on UV and visible emission bands in the co doped systems at two different sintering temperatures, indicating the existence of defects in the form of oxygen vacancies. While the TM: TM co doped samples of ZnO exhibit ferromagnetism at room temperature, the TM: RE co doped samples show paramagnetic behaviour. The magnetic behaviours observed are supported by results from Electron Spin resonance (ESR) study; which shows sharp resonance peaks with considerable line width (∆H) and g values more than 2. Such values are usually found due to the presence of an internal field inside the system giving rise to the shift of resonance field towards the lower field. The g values in this range are assigned to the unpaired electrons trapped in oxygen vacancies. TM: TM co doped ZnO samples exhibit low field absorption peaks in their ESR spectra, which is a new interesting observation. We emphasize that the interesting observations reported in this paper may be considered for the improved futuristic applications of ZnO based materials.

Keywords: co-doping, electro spin resonance, microwave absorption, spintronics

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Authors: Yu-Kuei Hsu, Ying-Chu Chen, Yan-Gu Lin

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The hierarchical Cu2S nano structural film is successfully fabricated via an electroplated ZnO nanorod array as a template and subsequently chemical solution process for the growth of Cu2S in the application of surface-enhanced Raman scattering (SERS) detection. The as-grown Cu2S nano structures were thermally treated at temperature of 150-300 oC under nitrogen atmosphere to improve the crystal quality and unexpectedly induce the Cu nano particles on surface of Cu2S. The structure and composition of thermally treated Cu2S nano structures were carefully analyzed by SEM, XRD, XPS, and XAS. Using 4-aminothiophenol (4-ATP) as probing molecules, the SERS experiments showed that the thermally treated Cu2S nano structures exhibit excellent detecting performance, which could be used as active and cost-effective SERS substrate for ultra sensitive detecting. Additionally, this novel hierarchical SERS substrates show good reproducibility and a linear dependence between analyte concentrations and intensities, revealing the advantage of this method for easily scale-up production.

Keywords: cuprous sulfide, copper, nanostructures, surface-enhanced raman scattering

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Authors: Yu-Kuei Hsu, Yan-Gu Lin

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A facile and simple fabrication of copper(II) oxide (CuO) nanosheet on copper foil as nanoelectrode for H2O2 sensing application was proposed in this study. The spontaneous formation of CuO nanosheets by immersing the copper foil into 0.1 M NaOH aqueous solution for 48 hrs was carried out at room temperature. The sheet-like morphology with several ten nanometers in thickness and ~500 nm in width was observed by SEM. Those nanosheets were confirmed the monoclinic-phase CuO by the structural analysis of XRD and Raman spectra. The directly grown CuO nanosheets film is mechanically stable and offers an excellent electrochemical sensing platform. The CuO nanosheets electrode shows excellent electrocatalytic response to H2O2 with significantly lower overpotentials for its oxidation and reduction and also exhibits a fast response and high sensitivity for the amperometric detection of H2O2. The novel spontaneously grown CuO nanosheets electrode is readily applicable to other analytes and has great potential applications in the electrochemical detection.

Keywords: CuO, nanosheets, H2O2 detection, Cu foil

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Authors: Asli Beyler Çi̇ği̇l, Memet Vezi̇r Kahraman

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Organic–inorganic hybrids have become an effective source of advanced materials because they combine the advantages of both the organic moiety such as flexibility, low dielectric constant, and processability, and inorganic moiety as rigidity, strength, durability, and thermal stability. By incorporating cross-linkable side chains, the hybrid materials can be made photosensitive and UV curable, which offers many advantages including low processing temperature, low equipment cost and compatibility. In this study, uv-curable organic-inorganic hybrid material, which was contained surface modified polyaniline particles (PANI), was prepared. PANI surface photografted with hydroxy ethyl methacrylate (HEMA) to produce hydroxyl groups. Hydroxyl functionalized PANI/HEMA was acrylated using isocyanato ethyl methacrylate (IEM) in order to improve the dispersion and interfacial interaction in composites. UV-curable formulation was prepared by mixing the surface modified PANI, polyethylene glycol diacrylate (PEGDA), trimethylolpropane triacrylate (TMPTA), hydrolized 3- methacryloxypropyltrimethoxysilane (hyd. MEMO) and photoinitiator. Chemical structure of nano-hybrid material was characterized by FTIR. FTIR spectra showed that the photografting of PANI was prepared successfully. Thermal properties of the nano-hybrid material were determined by thermogravimetric analysis (TGA). The morphology of the nano-hybrid material was performed by scanning electron microscopy (SEM).

Keywords: polyaniline, photograft, sol-gel, uv-curable polymer

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

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In this present work, CoFe2-xNdxO4 (0.0 ≤ x ≥0.1) spinel ferrite nanoparticles were synthesized by starch-assisted sol-gel auto-combustion method. Powder X-ray diffraction patterns were revealed the formation of cubic spinel ferrite with the signature of NdFeO3 phase at higher Nd3+ concentration. The field emission scanning electron microscopy study demonstrated the spherical nanoparticle in the size range between 5-15 nm. Raman and Fourier Transform Infrared spectra supported the formation of the spinel ferrite structure in the nanocrystalline form. The X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of Co2+ and Fe3+ at octahedral as well as a tetrahedral site in CoFe2-xNdxO4 nanoparticles. The change in magnetic properties with a variation of concentration of Nd3+ ions in cobalt ferrite nanoparticles was observed.

Keywords: nanoparticles, spinel ferrites, sol-gel auto-combustion method, CoFe2-xNdxO4

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

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

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

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Authors: W. Ketren, J. Wannapeera, Z. Heishun, A. Ryuichi, K. Toshiteru, M. Kouichi, O. Hideaki

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Degradative solvent extraction is the method developed for biomass upgrading by dewatering and fractionation of biomass under the mild condition. However, the conversion mechanism of the degradative solvent extraction method has not been fully understood so far. The rice straw was treated in 1-methylnaphthalene (1-MN) at a different solvent-treatment temperature varied from 250 to 350 ^oC with the residence time for 60 min. The liquid membrane-Fourier Transform Infrared Spectroscopy (FTIR) technique is applied to study the processing mechanism in-depth without separation of the solvent. It has been found that the strength of the oxygen-hydrogen stretching  (3600-3100 cm^-1) decreased slightly with increasing temperature in the range of 300-350 ^oC. The decrease of the hydroxyl group in the solvent soluble suggested dehydration reaction taking place between 300 and 350 ^oC. FTIR spectra in the carbonyl stretching region (1800-1600 cm^-1) revealed the presence of esters groups, carboxylic acid and ketonic groups in the solvent-soluble of biomass. The carboxylic acid increased in the range of 200 to 250 ^oC and then decreased. The prevailing of aromatic groups showed that the aromatization took place during extraction at above 250 ^oC. From 300 to 350 ^oC, the carbonyl functional groups in the solvent-soluble noticeably decreased. The removal of the carboxylic acid and the decrease of esters into the form of carbon dioxide indicated that the decarboxylation reaction occurred during the extraction process.

Keywords: biomass waste, degradative solvent extraction, mechanism, upgrading

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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: Issam Derkaoui, Mohammed Khenfouch, Bakang M. Mothudi, Malik Maaza, Izeddine Zorkani, Anouar Jorio

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Transition metal oxides nanoparticles with different morphologies have attracted a lot of attention recently owning to their distinctive geometries, and demonstrated promising electrical properties for various applications. In this paper, we discuss the time and annealing effects on the structural and electrical properties of vanadium oxides nanoparticles (VO-NPs) prepared by microwave method. In this sense, transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman Spectroscopy, Ultraviolet-visible absorbance spectra (Uv-Vis) and electrical conductivity were investigated. Hence, the annealing state and the time are two crucial parameters for the improvement of the optoelectronic properties. The use of these nanostructures is promising way for the development of technological applications especially for energy storage devices.

Keywords: Vanadium oxide, Microwave, Electrical conductivity, Optoelectronic properties

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Authors: D. P. Evdokimov, A. N. Kirichenko, V. D. Blank, V. N. Denisov, B. A. Kulnitskiy

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In this study we investigated the stability of polyhedral carbon onions under influence of shear deformation and high pressures above 43 GPa by means of by transmission electron microscopy (TEM) and Raman spectroscopy (RS). It was found that at pressures up to 29 GPa and shear deformations of 40 degrees the onions are stable. At shear deformation applying at pressures above 30 GPa carbon onions collapsed with formation of amorphous carbon. At pressures above 43 GPa diamond-like carbon (DLC) was obtained.

Keywords: carbon onions, Raman spectroscopy, transmission electron spectroscopy

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Authors: Y. Hamaizi, H. Triki, A. El-Akrmi

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In this paper, the reflection spectra, group delay and dispersion of a uniform fiber Bragg grating (FBG) are obtained. FBGs with two types of apodized variations of the refractive index were modeled to show how the side-lobes can be suppressed. Apodization techniques are used to get optimized reflection spectra. The simulation is based on solving coupled mode equations together with the transfer matrix method.

Keywords: fiber bragg gratings, coupled-mode theory, reflectivity, apodization

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Authors: Surendra Kumar Gautam, Mahesh Dhungana

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Magnesium oxide nanoparticles (MgO NPs) are less toxic to humans and the environment as compared to other metal oxide nanoparticles. Various conventional chemical and physical methods are used for synthesis whose toxicity level is high and highly expensive. As the best alternative, phyto-assisted synthesis has emerged, which uses extracts from plant parts for the synthesis of nanoparticles. Here, we report the synthesis of MgO nanoparticles with the assistance of beetroot extract and leaf extract of P. guajava and A. adenophora. The synthesized MgO NPs were characterized by X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), and UV-visible spectroscopy. X-ray analysis for the broadening of peaks was used to evaluate the crystallite size and lattice strain using Debye-Scherer and Williamson–Hall method. The results of crystallite size obtained by both methods are in close proximity. The crystallite size obtained by the Williamson-Hall method seems more accurate, with values being 8.1 nm and 13.2 nm for beetroot MgO NPs and P. guajava MgO NPs, respectively. The FT-IR spectroscopy revealed the dominance of chemical bonds as well as functional groups on MgO NPs surfaces. The UV-visible absorption spectra of MgO NPs were found to be 310 nm, 315 nm, and 315 nm for beetroot, P. guajava, and A. adenophora leaf extract, respectively. Among the three samples, beetroot-mediated MgO NPs were effective antibacterial against both gram-positive and Gram-negative bacteria. In addition, synthesized MgO NPs also show significant antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl radical. Further, beetroot MgO NPs showed the highest photocatalytic activity of about 91% in comparison with other samples.

Keywords: MgO NPs, XRD, FTIR, antibacterial, antioxidant and photocatalytic activity

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Authors: Aarti Muley, S. J. Dhoblae

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CaF₂ and BaF₂ doped with cerium were prepared by slow precipitation method with different molar concentration and different cerium concentration. Both the samples were also prepared by direct method for comparison. The XRD of BaF₂:Ce shows that it crystallizes to BCC structure. The peak matches with JCPDS file no. 4-0452. Also, The XRD pattern of CaF₂:Ce matches well with the JCPDS file number 75- 0363 and crystallized to BCC phase. In CaF₂, the double-humped photoluminescence spectra were observed at 320nm and 340nm when the sample was prepared by the direct precipitation method, and the ratio between these peaks is unity. However when the sample prepared by slow precipitation method the double-humped emission spectra of CaF₂:Ce was observed at 323nm and 340nm. The ratio between these peaks is 0.58, and the optimum concentration is obtained for 0.1 molar CaF₂ with Ce concentration 1.5%. When the cerium concentration is increased by 2% the peak at 323nm vanishes, and the emission was observed at 342nm with the shoulder at 360nm. In this case, the intensity reduces drastically. The excitation is observed at 305nm with a small peak at 254nm. One molar BaF₂ doped with 0.1% of cerium was synthesized by direct precipitation method gives double humped spectra at 308nm and 320nm, when it is prepared with slow precipitation method with the cerium concentration 0.05m%, 0.1m%, 0.15m%, 0.2m% the broad emission is observed around 325nm with the shoulder at 350nm. The excitation spectra are narrow and observed at 290nm. As the percentage of cerium is increased further again shift is observed. The emission spectra were observed at 360nm with a small peak at 330nm. The phenomenon of shifting of emission spectra at low concentration of cerium can directly relate with the particle size and reported for nanomaterials also.

Keywords: calcium fluoride, barium fluoride, photoluminescence, slow precipitation method

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Authors: Mohammad Arifin, Huda Abdullah, Norshafadzila Mohammad Naim

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The fabricated PANI-(SnO₂, ZnO)/rGO nanocomposite thin films for the E. coli bacteria sensor were investigated. The nanocomposite thin films were prepared by the sol-gel method and deposited on the glass substrate using the spin-coating technique. The internal structure and surface morphology of the thin films have been analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and atomic force microscopy (AFM). The optical properties of the films were investigated by UV-Vis spectroscopy, Raman spectroscopy, and Fourier transform infrared spectroscopy (FTIR). The sensitivity performance was identified by measuring the changing conductivity before and after the incubation of E. coli bacteria using current-voltage (I-V) and cyclic voltammetry (C-V) measurements.

Keywords: PANI-(SnO₂, ZnO)/rGO, nanocomposite, bacteria sensor, thin films

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Authors: Anna Krukowska, Tomasz Klimczuk, Adriana Zaleska-Medynska

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Photoactive materials have attracted attention due to their potential application in the degradation of environmental pollutants to non-hazardous compounds in an eco-friendly route. Among semiconductor photocatalysts, tantalates such as potassium tantalate (KTaO3) is one of the excellent functional photomaterial. However, tantalates-based materials are less active under visible-light irradiation, the enhancement in photoactivity could be improved with the modification of opto-eletronic properties of KTaO3 by doping rare earth metal (Er) and further photodeposition of noble metal nanoparticles (Pt). Inclusion of rare earth element in orthorhombic structure of tantalate can generate one high-energy photon by absorbing two or more incident low-energy photons, which convert visible-light and infrared-light into the ultraviolet-light to satisfy the requirement of KTaO3 photocatalysts. On the other hand, depositions of noble metal nanoparticles on the surface of semiconductor strongly absorb visible-light due to their surface plasmon resonance, in which their conducting electrons undergo a collective oscillation induced by electric field of visible-light. Furthermore, the high dispersion of Pt nanoparticles, which will be obtained by photodeposition process is additional important factor to improve the photocatalytic activity. The present work is aimed to study the effect of photocatalytic process of the prepared Er-doped KTaO3 and further incorporation of Pt nanoparticles by photodeposition. Moreover, the research is also studied correlations between photocatalytic activity and physico-chemical properties of obtained Pt/Er-KTaO3 samples. The Er-doped KTaO3 microcomposites were synthesized by a hydrothermal method. Then photodeposition method was used for Pt loading over Er-KTaO3. The structural and optical properties of Pt/Er-KTaO3 photocatalytic were characterized using scanning electron microscope (SEM), X-ray diffraction (XRD), volumetric adsorption method (BET), UV-Vis absorption measurement, Raman spectroscopy and luminescence spectroscopy. The photocatalytic properties of Pt/Er-KTaO3 microcomposites were investigated by degradation of phenol in aqueous phase as model pollutant under visible and ultraviolet-light irradiation. Results of this work show that all the prepared photocatalysis exhibit low BET surface area, although doping of the bare KTaO3 with rare earth element (Er) presents a slight increase in this value. The crystalline structure of Pt/Er-KTaO3 powders exhibited nearly identical positions for the main peak at about 22,8o and the XRD pattern could be assigned to an orthorhombic distorted perovskite structure. The Raman spectra of obtained semiconductors confirmed demonstrating perovskite-like structure. The optical absorption spectra of Pt nanoparticles exhibited plasmon absorption band for main peaks at about 216 and 264 nm. The addition of Pt nanoparticles increased photoactivity compared to Er-KTaO3 and pure KTaO3. Summary optical properties of KTaO3 change with its doping Er-element and further photodeposition of Pt nanoparticles.

Keywords: heterogeneous photocatalytic, KTaO3 photocatalysts, Er3+ ion doping, Pt photodeposition

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Authors: A. G. Pershina, P. S. Postnikov, M. E. Trusova, D. O. Burlakova, A. E. Sazonov

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Invention of magnetic-fluorescent nanocomposites is a rapidly developing area of research. The magnetic-fluorescent nanocomposite attractiveness is connected with the ability of simultaneous management and control of such nanocomposites by two independent methods based on different physical principles. These nanocomposites are applied for the solution of various essential scientific and experimental biomedical problems. The aim of this research is development of principle approach to nanobiohybrid structures with magnetic and fluorescent properties design. The surface of carbon-coated iron nanoparticles (Fe@C) were covalently modified by 4-carboxy benzenediazonium tosylate. Recombinant fluorescent protein TagGFP2 (Eurogen) was obtained in E. coli (Rosetta DE3) by standard laboratory techniques. Immobilization of TagGFP2 on the nanoparticles surface was provided by the carbodiimide activation. The amount of COOH-groups on the nanoparticle surface was estimated by elemental analysis (Elementar Vario Macro) and TGA-analysis (SDT Q600, TA Instruments. Obtained nanocomposites were analyzed by FTIR spectroscopy (Nicolet Thermo 5700) and fluorescence microscopy (AxioImager M1, Carl Zeiss). Amount of the protein immobilized on the modified nanoparticle surface was determined by fluorimetry (Cary Eclipse) and spectrophotometry (Unico 2800) with the help of preliminary obtained calibration plots. In the FTIR spectra of modified nanoparticles the adsorption band of –COOH group around 1700 cm-1 and bands in the region of 450-850 cm-1 caused by bending vibrations of benzene ring were observed. The calculated quantity of active groups on the surface was equal to 0,1 mmol/g of material. The carbodiimide activation of COOH-groups on nanoparticles surface results to covalent immobilization of TagGFP2 fluorescent protein (0.2 nmol/mg). The success of immobilization was proved by FTIR spectroscopy. Protein characteristic adsorption bands in the region of 1500-1600 cm-1 (amide I) were presented in the FTIR spectrum of nanocomposite. The fluorescence microscopy analysis shows that Fe@C-TagGFP2 nanocomposite possesses fluorescence properties. This fact confirms that TagGFP2 protein retains its conformation due to immobilization on nanoparticles surface. Magnetic-fluorescent nanocomposite was obtained as a result of unique design solution implementation – the fluorescent protein molecules were fixed to the surface of superparamagnetic carbon-coated iron nanoparticles using original diazonium salts.

Keywords: carbon-coated iron nanoparticles, diazonium salts, fluorescent protein, immobilization

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Authors: Anika Zafiah M. Rus, Nur Munirah Abdullah, M. F. L. Abdullah

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The fabrication and characterization of composite films of graphite- bioepoxy is described. Free-standing thin films of ~0.1 mm thick are prepared using a simple solution mixing with mass proportion of 7/3 (bioepoxy/graphite) and drop casting at room temperature. Fourier transform infra-red spectroscopy (FTIR) and Ultraviolet-visible (UV-vis) spectrophotometer are performed to evaluate the changes in chemical structure and adsorption spectra arising with the increasing of graphite weight loading (wt.%) into the biopolymer matrix. The morphologic study shows a homogeneously dispersed and strong particle bonding between the graphite and the bioepoxy, with conductivity of the film 103 S/m, confirming the efficiency of the processes.

Keywords: absorbance peak, biopolymer, graphite- bioepoxy composites, particle bonding

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

Abstract:

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

Keywords: hydroxyapatite, substitution, characterization, XRD, FTIR

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Authors: Radka Králová, Libor Kvítek, Václav Ranc, Aleš Panáček, Radek Zbořil

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Surface–Enhanced Raman Scattering (SERS) is an optical spectroscopic technique with very good potential for sensitive detection of substances. In this research, active substrates with high enhancement were provided. Novel silver particles (nanostructures) with high roughened, flower–like morphology were prepared by reduction of cation complex [Ag(NH3)2]+ in presence of sodium borohydride as reducing agent and stabilized polyacrylic acid. The products were characterized by UV/VIS absorption spectrophotometry. Special shapes of silver particles were determined by scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM). Dispersions of this particle were put on fixed substrate to producing suitable layer for SERS. Adenine was applied as basic substance whose effect of enhancement on the layer of silver nanostructures was studied. By comparison with our work, the important influence of stabilizers, polyacrylic acid with various molecular weight and concentration, on the transfer of particles and formation of new structure was confirmed.

Keywords: metals, nanostructures, chemical reduction, Raman spectroscopy, optical properties

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Authors: Jai Prakash, Promod Kumar, Chantel Swart, J. H. Neethling, A. Janse van Vuuren, H. C. Swart

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Ag nanoparticles (NPs) have been used as functional nanomaterials due to their optical and antibacterial properties. Similarly, TiO2 photocatalysts have also been used as suitable nanomaterials for killing cancer cells, viruses and bacteria. Here, we report on multifunctional plasmonic Ag-TiO2 nano-biocomposite synthesized by the sol-gel technique and their optical, surface enhanced Raman scattering (SERS) and antibacterial activities. The as-prepared composites of Ag–TiO2 with different silver content and TiO2 nanopowder were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, energy-dispersed X-ray analysis (EDX), UV-vis and Raman spectroscopy. The Ag NPs were found to be uniformly distributed and strongly attached to the TiO2 matrix. The novel optical response of the Ag-TiO2 nanocomposites is due to the strong electric field from the surface plasmon excitation of the Ag NPs. The Raman spectrum of Ag-TiO2 nanocomposite was found to be enhanced as compared to TiO2. The enhancement of the low frequency band is evident. This indicates the SERS effect of the TiO2 NPs in close vicinity of Ag NPs. In addition, nanocomposites showed enhancement in the SERS signals of methyl orange (MO) dye molecules with increasing Ag content. The localized electromagnetic field from the surface plasmon excitation of the Ag NPs was responsible for the SERS signals of the TiO2 NPs and MO molecules. The antimicrobial effect of the Ag–TiO2 nanocomposites with different silver content and TiO2 nanopowder were carried out against the bacterium Staphylococcus aureus. The Ag–TiO2 composites showed antibacterial activity towards S. aureus with increasing Ag content as compared to the TiO2 nanopowder. These results foresee promising applications of the functional plasmonic metal−semiconductor based nanobiocomposites for both chemical and biological samples.

Keywords: metal-Semiconductor, nano-Biocomposites, anti-microbial activity, surface enhanced Raman scattering

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Authors: Mahamuda Sk, Srinivasa Rao Allam, Vijaya Prakash G.

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The different concentrations of Eu3+ ions doped in Oxy-fluoroborate glasses of composition 60 B2O3-10 BaF2-10 CaF2-15 CaF2- (5-x) Al2O3 -x Eu2O3 where x = 0.1, 0.5, 1.0 and 2.0 mol%, have been prepared by conventional melt quenching technique and are characterized through absorption and photoluminescence (PL), decay, color chromaticity and Confocal measurements. The absorption spectra of all the glasses consists of six peaks corresponding to the transitions 7F0→5D2, 7F0→5D1, 7F1→5D1, 7F1→5D0, 7F0→7F6 and 7F1→7F6 respectively. The experimental oscillator strengths with and without thermal corrections have been evaluated using absorption spectra. Judd-Ofelt (JO) intensity parameters (Ω2 and Ω4) have been evaluated from the photoluminescence spectra of all the glasses. PL spectra of all the glasses have been recorded at excitation wavelengths 395 nm (conventional excitation source) and 410 nm (diode laser) to observe the intensity variation in the PL spectra. All the spectra consists of five emission peaks corresponding to the transitions 5D0→7FJ (J = 0, 1, 2, 3 and 4). Surprisingly no concentration quenching is observed on PL spectra. Among all the glasses the glass with 2.0 mol% of Eu3+ ion concentration possesses maximum intensity for the transition 5D0→7F2 (612 nm) in bright red region. The JO parameters derived from the photoluminescence spectra have been used to evaluate the essential radiative properties such as transition probability (A), radiative lifetime (τR), branching ratio (βR) and peak stimulated emission cross-section (σse) for the 5D0→7FJ (J = 0, 1, 2, 3 and 4) transitions of the Eu3+ ions. The decay rates of the 5D0 fluorescent level of Eu3+ ions in the title glasses are found to be single exponential for all the studied Eu3+ ion concentrations. A marginal increase in lifetime of the 5D0 level has been noticed with increase in Eu3+ ion concentration from 0.1 mol% to 2.0 mol%. Among all the glasses, the glass with 2.0 mol% of Eu3+ ion concentration possesses maximum values of branching ratio, stimulated emission cross-section and quantum efficiency for the transition 5D0→7F2 (612 nm) in bright red region. The color chromaticity coordinates are also evaluated to confirm the reddish luminescence from these glasses. These color coordinates exactly fall in the bright red region. Confocal images also recorded to confirm reddish luminescence from these glasses. From all the obtained results in the present study, it is suggested that the glass with 2.0 mol% of Eu3+ ion concentration is suitable to emit bright red color laser.

Keywords: Europium, Judd-Ofelt parameters, laser, luminescence

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Authors: S. Mohamadi, T. Boudina, A. Rouabeh, A. Seridi

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Equivalent linear and non-linear ground response analyses are conducted at many representative sites at the mosque of Algeria, to compare the free field acceleration spectra with local code of practice. Spectral Analysis of Surface Waves (SASW) technique was adopted to measure the in-situ shear wave velocity profile at the representative sites. The seismic movement imposed on the rock is the NS component of Keddara station recorded during the earthquake in Boumerdes 21 May 2003. The site-specific elastic design spectra for each site are determined to further obtain site specific non-linear acceleration spectra. As a case study, the results of site-specific evaluations are presented for two building sites (site of minaret and site of the prayer hall) to demonstrate the influence of local geological conditions on ground response at Algerian sites. A comparison of computed response with the standard code of practice being used currently in Algeria for the seismic zone of Algiers indicated that the design spectra is not able to capture site amplification due to local geological conditions.

Keywords: equivalent linear, non-linear, ground response analysis, design response spectrum

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Authors: Chieh-Chun Chang, Cheng-Ting Shih, Yan-Lin Liu, Shu-Jun Chang, Jay Wu

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With the widespread use of digital mammography (DM), radiation dose evaluation of breasts has become important. X-ray spectra are one of the key factors that influence the absorbed dose of glandular tissue. In this study, we estimated the X-ray spectrum of DM using the expectation maximization (EM) algorithm with the transmission measurement data. The interpolating polynomial model proposed by Boone was applied to generate the initial guess of the DM spectrum with the target/filter combination of Mo/Mo and the tube voltage of 26 kVp. The Monte Carlo N-particle code (MCNP5) was used to tally the transmission data through aluminum sheets of 0.2 to 3 mm. The X-ray spectrum was reconstructed by using the EM algorithm iteratively. The influence of the initial guess for EM reconstruction was evaluated. The percentage error of the average energy between the reference spectrum inputted for Monte Carlo simulation and the spectrum estimated by the EM algorithm was -0.14%. The normalized root mean square error (NRMSE) and the normalized root max square error (NRMaSE) between both spectra were 0.6% and 2.3%, respectively. We conclude that the EM algorithm with transmission measurement data is a convenient and useful tool for estimating x-ray spectra for DM in clinical practice.

Keywords: digital mammography, expectation maximization algorithm, X-Ray spectrum, X-Ray

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Authors: Andreas Kerstan, Darren Robey, Wesam Alvan, David Troiani

Abstract:

Over the last 3.5 years, Quantum Cascade Lasers (QCL) technology has become increasingly important in infrared (IR) microscopy. The advantages over fourier transform infrared (FTIR) are that large areas of a few square centimeters can be measured in minutes and that the light intensive QCL makes it possible to obtain spectra with excellent S/N, even with just one scan. A firmly established solution of the laser direct infrared imaging (LDIR) 8700 is the analysis of microplastics. The presence of microplastics in the environment, drinking water, and food chains is gaining significant public interest. To study their presence, rapid and reliable characterization of microplastic particles is essential. Significant technical hurdles in microplastic analysis stem from the sheer number of particles to be analyzed in each sample. Total particle counts of several thousand are common in environmental samples, while well-treated bottled drinking water may contain relatively few. While visual microscopy has been used extensively, it is prone to operator error and bias and is limited to particles larger than 300 µm. As a result, vibrational spectroscopic techniques such as Raman and FTIR microscopy have become more popular, however, they are time-consuming. There is a demand for rapid and highly automated techniques to measure particle count size and provide high-quality polymer identification. Analysis directly on the filter that often forms the last stage in sample preparation is highly desirable as, by removing a sample preparation step it can both improve laboratory efficiency and decrease opportunities for error. Recent advances in infrared micro-spectroscopy combining a QCL with scanning optics have created a new paradigm, LDIR. It offers improved speed of analysis as well as high levels of automation. Its mode of operation, however, requires an IR reflective background, and this has, to date, limited the ability to perform direct “on-filter” analysis. This study explores the potential to combine the filter with an infrared reflective surface filter. By combining an IR reflective material or coating on a filter membrane with advanced image analysis and detection algorithms, it is demonstrated that such filters can indeed be used in this way. Vibrational spectroscopic techniques play a vital role in the investigation and understanding of microplastics in the environment and food chain. While vibrational spectroscopy is widely deployed, improvements and novel innovations in these techniques that can increase the speed of analysis and ease of use can provide pathways to higher testing rates and, hence, improved understanding of the impacts of microplastics in the environment. Due to its capability to measure large areas in minutes, its speed, degree of automation and excellent S/N, the LDIR could also implemented for various other samples like food adulteration, coatings, laminates, fabrics, textiles and tissues. This presentation will highlight a few of them and focus on the benefits of the LDIR vs classical techniques.

Keywords: QCL, automation, microplastics, tissues, infrared, speed

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