Search results for: X-ray photoelectron spectroscopy

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: Lucky Malise, Hilary Rutto, Tumisang Seodigeng

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The use of tires in automobiles is very important in the automobile industry. However, there is a serious environmental problem concerning the disposal of these rubber tires once they become worn out. The main aim of this study was to prepare activated carbon from waste tire pyrolysis char by impregnating KOH on pyrolytic char. Adsorption studies on lead onto chemically activated carbon was carried out using response surface methodology. The effect of process parameters such as temperature (°C), adsorbent dosage (g/1000ml), pH, contact time (minutes) and initial lead concentration (mg/l) on the adsorption capacity were investigated. It was found that the adsorption capacity increases with an increase in contact time, pH, temperature and decreases with an increase in lead concentration. Optimization of the process variables was done using a numerical optimization method. Fourier Transform Infrared Spectra (FTIR) analysis, XRay diffraction (XRD), Thermogravimetric analysis (TGA) and scanning electron microscope was used to characterize the pyrolytic carbon char before and after activation. The optimum points 1g/ 100 ml for adsorbent dosage, 7 for pH value of the solution, 115.2 min for contact time, 100 mg/l for initial metal concentration, and 25°C for temperature were obtained to achieve the highest adsorption capacity of 93.176 mg/g with a desirability of 0.994. Fourier Transform Infrared Spectra (FTIR) analysis and Thermogravimetric analysis (TGA) show the presence of oxygen-containing functional groups on the surface of the activated carbon produced and that the weight loss taking place during the activation step is small.

Keywords: waste tire pyrolysis char, chemical activation, central composite design (CCD), adsorption capacity, numerical optimization

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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: Maksudur Rahman Khan, Kar Min Chan, Huei Ruey Ong, Chin Kui Cheng, Wasikur Rahman

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Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However, the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol-gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The as-prepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

Keywords: microbial fuel cell, oxygen reduction reaction, Pt/MnO2, palm oil mill effluent, polarization curve

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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Authors: Mannan Malik Muhammad Naeem, Jeong Myung Yung

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Functional near infrared spectroscopy (fNIRS) has a favorable position in non-invasive brain imaging techniques. The concentration change of oxygenated hemoglobin and de-oxygenated hemoglobin during particular cognitive activity is the basis for this neuro-imaging modality. Two wavelengths of near-infrared light can be used with modified Beer-Lambert law to explain the indirect status of neuronal activity inside brain. The temporal resolution of fNIRS is very good for real-time brain computer-interface applications. The portability, low cost and an acceptable temporal resolution of fNIRS put it on a better position in neuro-imaging modalities. In this study, an optimization model for impulse response function has been used to estimate/predict initial dip using fNIRS data. In addition, the activity strength parameter related to motor based cognitive task has been analyzed. We found an initial dip that remains around 200-300 millisecond and better localize neural activity.

Keywords: fNIRS, brain-computer interface, optimization algorithm, adaptive signal processing

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Authors: Damandeep Kaur, O.P. Pandey, M.S. Reddy

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In the present research, bio-synthesisation of silica particles has been carried out successfully. For this purpose, agriculture waste rice husk (RH) has been utilized. Among several types of agriculture waste, RH is considered to be cost-effective and easily accessible. In the present investigation, a chemical approach has been followed to extract silica nanoparticles. X-Ray Diffraction (XRD) patterns indicated the amorphous nature of silica at lower temperature range. Silica and other mineral contents have been found using energy dispersive spectroscopy (EDS). Morphological and structural studies have been carried out with the use of Field Emission Scanning Electron Microscopy (FE-SEM) and Fourier Transform Infrared Transmission (FTIR) spectroscopy. Further, extracted silica from RH has been used for preparation of the glasses. The appearance of broad humps in XRD patterns confirmed the amorphous nature of prepared glasses. These glasses exhibited enhanced antibacterial effect against both Gram-positive and Gram-negative bacteria. The as-synthesized glass samples can be further used for physical and structural studies for drug loading applications.

Keywords: rice husk, biosynthesized silica, bioactive glasses, antibacterial studies

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Authors: Suhas Kadam, Vishal Chandanshive, Niraj Rane, Sanjay Govindwar

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Fimbristylis dichotoma, Ammannia baccifera, and their co-plantation consortium FA were found to degrade methyl orange, simulated dye mixture, and real textile effluent. Wild plants of Fimbristylis dichotoma and Ammannia baccifera with equal biomass showed 91 and 89% decolorization of methyl orange within 60 h at a concentration of 50 ppm, while 95% dye removal was achieved by consortium FA within 48 h. Floating phyto-beds with co-plantation (Fimbristylis dichotoma and Ammannia baccifera) for the treatment of real textile effluent in a constructed wetland was observed to be more efficient and achieved 79, 72, 77, 66 and 56% reductions in ADMI color value, chemical oxygen demand, biological oxygen demand, total dissolve solid and total suspended solid of textile effluent, respectively. High performance thin layer chromatography, gas chromatography-mass spectroscopy, Fourier transform infrared spectroscopy, Ultra violet-Visible spectroscopy and enzymatic assays confirmed the phytotransformation of parent dye in the new metabolites. T-RFLP analysis of rhizospheric bacteria of Fimbristylis dichotoma, Ammannia baccifera, and consortium FA revealed the presence of 88, 98 and 223 genera which could have been involved in dye removal. Toxicity evaluation of products formed after phytotransformation of methyl orange by consortium FA on bivalves Lamellidens marginalis revealed less damage in the gills architecture when analyzed histologically. Toxicity measurement by Random Amplification of Polymorphic DNA (RAPD) technique revealed normal banding pattern in treated methyl orange sample suggesting less toxic nature of phytotransformed dye products.

Keywords: constructed wetland, phyto-bed, textile effluent, phytoremediation

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Authors: Zakaria Ahmed, Khaled Charradi, Sherif M. A. S. Keshk, Radhouane Chtourou

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Sulfonated poly ether ether ketone (SPEEK) with a low sulfonation degree was blended using nanofiller Layered Double Hydroxide (LDH, Mg2AlCl) /sepiolite nanostructured material as additive to use as an electrolyte membrane for fuel cell application. Characterization assessments, i.e., mechanical stability, thermal gravimetric analysis, ion exchange capability, swelling properties, water uptake capacities, electrochemical impedance spectroscopy analysis, and Fourier transform infrared spectroscopy (FTIR) of the composite membranes were conducted. The presence of LDH/sepiolite nanoarchitecture material within SPEEK was found to have the highest water retention and proton conductivity value at high temperature rather than LDH/SPEEK and pristine SPEEK membranes.

Keywords: SPEEK, sepiolite clay, LDH clay, proton exchange membrane

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Authors: Shajaratuldur Ismail, Nurlidia Mansor, Zakaria Man

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Thermoplastic starch (TPS) plasticized by 1-ethyl-3-methylimidazolium acetate [Emim][OAc] were obtained through gelatinization process. The gelatinization process occurred in the presence of water and [Emim][OAc] as plasticizer at high temperature (90˚C). The influence of [Emim][OAc] and water on the gelatinization and interactions with starch have been studied over a range of compositions. The homogenous mass was obtained for the samples containing 35, 40 and 43.5 % of water contents which showed that water plays important role in gelatinization process. Detailed IR spectroscopy analysis showed decrease in hydrogen bonding intensity and strong interaction between acetate anion in [Emim][OAc] and starch hydroxyl groups in the presence of [Emim][OAc]. Starch-[Emim][OAc]-water mixture at 10-3-8.7 presented homogenous mass, less hydrogen bonding intensity and strong interaction between acetate anion in [Emim][OAc] and starch hydroxyl groups.

Keywords: starch, ionic liquid, 1-ethyl-3-methylimidazolium acetate, plasticizer, gelatinization, IR spectroscopy

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Authors: A. Hamam, D. Oukil, A. Dib, L. Makhloufi

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The aim of this work is to synthesize modified Polypyrrole films (PPy) containing nanoparticles of copper oxides onto a non conducting cellulosic substrate. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is carried out using FeCl3 as an oxidant and Pyrrole as monomer. Different parameters were optimized (monomer concentration, duration of the experiment, nature of supporting electrolyte, temperature, etc.) in order to obtain films with different thickness and different morphologies. Thickness and topography of different PPy deposits were estimated by a profilometer apparatus. The electrochemical reactivity of the obtained electrodes were tested by cyclic voltammetry technique (CV) and electrochemical impedance spectroscopy (EIS). Secondly, the modification of the PPy film surface by incorporation of copper oxide nanonoparticles is conducted by applying a galvanostatic procedure from CuCl2 solution. Surface characterization has been carried out using scanning microscope (SEM) coupled with energy dispersive X-ray analysis (EDX), Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis showed the presence of the copper oxide nanoparticles (CuO) in the polymer films with dimensions less than 50 nm.

Keywords: polypyrrole, modified electrode, cellulosic substrate, copper oxide

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Authors: C. Fornacelli, P. Colomban, E. Mugnaioli, I. Memmi Turbanti

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When semiconductor particles are reduced in scale to nanometer dimension, their optical and electro-optical properties strongly differ from those of bulk crystals of the same composition. Since sampling is often not allowed concerning cultural heritage artefacts, the potentialities of two non-invasive techniques, such as Raman and Fiber Optic Reflectance Spectroscopy (FORS), have been investigated and the results of the analysis on some original glasses of different colours (from yellow to orange and deep red) and periods (from the second decade of the 20th century to present days) are reported in the present study. In order to evaluate the potentialities of the application of non-invasive techniques to the investigation of the structure and distribution of nanoparticles dispersed in a glass matrix, Scanning Electron Microscopy (SEM) and energy-disperse spectroscopy (EDS) mapping, together with Transmission Electron Microscopy (TEM) and Electron Diffraction Tomography (EDT) have also been used. Raman spectroscopy allows a fast and non-destructive measure of the quantum dots composition and size, thanks to the evaluation of the frequencies and the broadening/asymmetry of the LO phonons bands, respectively, though the important role of the compressive strain arising from the glass matrix and the possible diffusion of zinc from the matrix to the nanocrystals should be taken into account when considering the optical-phonons frequency values. The incorporation of Zn has been assumed by an upward shifting of the LO band related to the most abundant anion (S or Se), while the role of the surface phonons as well as the confinement-induced scattering by phonons with a non-zero wavevectors on the Raman peaks broadening has been verified. The optical band gap varies from 2.42 eV (pure CdS) to 1.70 eV (CdSe). For the compositional range between 0.5≤x≤0.2, the presence of two absorption edges has been related to the contribution of both pure CdS and the CdSxSe1-x solid solution; this particular feature is probably due to the presence of unaltered cubic zinc blende structures of CdS that is not taking part to the formation of the solid solution occurring only between hexagonal CdS and CdSe. Moreover, the band edge tailing originating from the disorder due to the formation of weak bonds and characterized by the Urbach edge energy has been studied and, together with the FWHM of the Raman signal, has been assumed as a good parameter to evaluate the degree of topological disorder. SEM-EDS mapping showed a peculiar distribution of the major constituents of the glass matrix (fluxes and stabilizers), especially concerning those samples where a layered structure has been assumed thanks to the spectroscopic study. Finally, TEM-EDS and EDT were used to get high-resolution information about nanocrystals (NCs) and heterogeneous glass layers. The presence of ZnO NCs (< 4 nm) dispersed in the matrix has been verified for most of the samples, while, for those samples where a disorder due to a more complex distribution of the size and/or composition of the NCs has been assumed, the TEM clearly verified most of the assumption made by the spectroscopic techniques.

Keywords: CdSxSe1-x, EDT, glass, spectroscopy, TEM-EDS

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Authors: V. Pérez-Herranz, C. González-Buch, E. M. Ortega, S. Mestre

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In this work new macroporous Ni electrodes modified with Au nanoparticles for hydrogen production have been developed. The supporting macroporous Ni electrodes have been obtained by means of the electrodeposition at high current densities. Then, the Au nanoparticles were synthesized and added to the electrode surface. The electrocatalytic behaviour of the developed electrocatalysts was studied by means of pseudo-steady-state polarization curves, electrochemical impedance spectroscopy (EIS) and hydrogen discharge curves. The size of the Au synthetized nanoparticles shows a monomodal distribution, with a very sharp band between 10 and 50 nm. The characteristic parameters d10, d50 and d90 were 14, 20 and 31 nm respectively. From Tafel polarization data has been concluded that the Au nanoparticles improve the catalytic activity of the developed electrodes towards the HER respect to the macroporous Ni electrodes. EIS permits to obtain the electrochemically active area by means of the roughness factor value. All the developed electrodes show roughness factor values in the same order of magnitude. From the activation energy results it can be concluded that the Au nanoparticles improve the intrinsic catalytic activity of the macroporous Ni electrodes.

Keywords: Au nano particles, hydrogen evolution reaction, porous Ni electrodes, electrochemical impedance spectroscopy

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Authors: Gaurav Verma

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Organoclay loaded (0-5 weight %) polyester-urethane (PU) coatings were prepared with a branched hydroxyl-bearing polyester and an aliphatic poly-isocyanate. TEM micrographs show partial exfoliation and intercalation of clay platelets in organoclay-polyester dispersions. AFM surface images reveals that the PU hard domains tend to regularise and also self-organise into spherical shapes of sizes 50 nm (0 wt %), 60 nm (2 wt %) and 190 nm (4 wt %) respectively. IR analysis shows that PU chains have increasing tendency to interact with exfoliated clay platelets through hydrogen bonding. This interaction strengthens inter-chain linkages in PU matrix and hence improves anti-ageing properties. 1000 hours of accelerated weathering was evaluated by ATR spectroscopy, while yellowing and overall discoloration was quantified by the Δb* and ΔE* values of the CIELab colour scale. Post-weathering surface properties also showed improvement as the loss of thickness and reduction in gloss in neat PU was 25% and 42%; while it was just 3.5% and 14% respectively for the 2 wt% nanocomposite coating. This work highlights the importance of modifying surface and bulk properties of PU coatings at nanoscale, which led to improved performance in accelerated weathering conditions.

Keywords: coatings, AFM, ageing, spectroscopy

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Authors: Abdalla A. Elbashir, Maali Saad Mokhtar, FakhrEldin O. Suliman

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The inclusion complexes of imazapyr (IMA) with 2-hydroxypropyl(β/γ) cyclodextrins (HP β/γ-CD), have been studied in aqueous media and in the solid state. In this work, fluorescence spectroscopy, electrospray-ionization mass spectrometry (ESI-MS), and HNMR were used to investigate and characterize the inclusion complexes of IMA with the cyclodextrins in solutions. The solid-state complexes were obtained by freeze-drying and were characterized by Fourier transform infrared spectroscopy (FTIR), and powder X-ray diffraction (PXRD). The most predominant complexes of IMA with both hosts are the 1:1 guest: host complexes. The association constants of IMA-HP β-CD and IMA-HP γ -CD were 115 and 215 L mol⁻¹, respectively. Molecular dynamic (MD) simulations were used to monitor the mode of inclusion and also to investigate the stability of these complexes in aqueous media at atomistic levels. The results obtained have indicated that these inclusion complexes are highly stable in aqueous media, thereby corroborating the experimental results. Additionally, it has been demonstrated that in addition to hydrophobic interactions and van der Waals interactions the presence of hydrogen bonding interactions of the type H---O and CH---O between the guest and the host have enhanced the stability of these complexes remarkably.

Keywords: imazapyr, inclusion complex, herbicides, 2-hydroxypropyl-β/γ-cyclodextrin

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Authors: Ahmed Abdrabou, Medhat Abdalla

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The studied stele dates back to Third Intermediate Period (1075-664) B.C in an ancient Egypt. It is made of wood and covered with painted gesso layers. This study aims to use a combination of multi spectral imaging {visible, infrared (IR), Visible-induced infrared luminescence (VIL), Visible-induced ultraviolet luminescence (UVL) and ultraviolet reflected (UVR)}, along with portable x-ray fluorescence in order to map and identify the pigments as well as to provide a deeper understanding of the painting techniques. Moreover; the authors were significantly interested in the identification of wood species. Multispectral imaging acquired in 3 spectral bands, ultraviolet (360-400 nm), visible (400-780 nm) and infrared (780-1100 nm) using (UV Ultraviolet-induced luminescence (UVL), UV Reflected (UVR), Visible (VIS), Visible-induced infrared luminescence (VIL) and Infrared photography. False color images are made by digitally editing the VIS with IR or UV images using Adobe Photoshop. Optical Microscopy (OM), potable X-ray fluorescence spectroscopy (p-XRF) and Fourier Transform Infrared Spectroscopy (FTIR) were used in this study. Mapping and imaging techniques provided useful information about the spatial distribution of pigments, in particular visible-induced luminescence (VIL) which allowed the spatial distribution of Egyptian blue pigment to be mapped and every region containing Egyptian blue, even down to single crystals in some instances, is clearly visible as a bright white area; however complete characterization of the pigments requires the use of p. XRF spectroscopy. Based on the elemental analysis found by P.XRF, we conclude that the artists used mixtures of the basic mineral pigments to achieve a wider palette of hues. Identification of wood species Microscopic identification indicated that the wood used was Sycamore Fig (Ficus sycomorus L.) which is recorded as being native to Egypt and was used to make wooden artifacts since at least the Fifth Dynasty.

Keywords: polychrome wooden stele, multispectral imaging, IR luminescence, Wood identification, Sycamore Fig, p-XRF

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Authors: Shahnaz Ashrafpour, Tahereh Tohidi Moghadam, Bijan Ranjbar

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Identifying the nature of protein-nanoparticle interactions and favored binding sites is an important issue in functional characterization of biomolecules and their physiological responses. Herein, interaction of silver nanoparticles with lysozyme as a model protein has been monitored via fluorescence spectroscopy. Formation of complex between the biomolecule and silver nanoparticles (AgNPs) induced a steady state reduction in the fluorescence intensity of protein at different concentrations of nanoparticles. Tryptophan fluorescence quenching spectra suggested that silver nanoparticles act as a foreign quencher, approaching the protein via this residue. Analysis of the Stern-Volmer plot showed quenching constant of 3.73 µM−1. Moreover, a single binding site in lysozyme is suggested to play role during interaction with AgNPs, having low affinity of binding compared to gold nanoparticles. Unfolding studies of lysozyme showed that complex of lysozyme-AgNPs has not undergone structural perturbations compared to the bare protein. Results of this effort will pave the way for utilization of sensitive spectroscopic techniques for rational design of nanobiomaterials in biomedical applications.

Keywords: nanocarrier, nanoparticles, surface plasmon resonance, quenching fluorescence

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Authors: Luxi He, Tianfang Zhang, Zhengbin He, Songlin Yi

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Heat treatment has been widely recognized for its effectiveness in enhancing the physicochemical properties of wood, including hygroscopicity and dimensional stability. Nonetheless, the non-negligible volumetric shrinkage and loss of mechanical strength resulting from heat treatment may diminish the wood recovery and its product value. In this study, tung oil was used to alleviate heat-induced shrinkage and reduction in mechanical properties of wood during heat treatment. Tung oil was chosen as a modifier because it is a traditional Chinese plant oil that has been widely used for over a thousand years to protect wooden furniture and buildings due to its biodegradable and non-toxic properties. The effects of different heating media (air, tung oil) and their effective treatment parameters (temperature, duration) on the changes in the physical properties (morphological characteristics, pore structures, micromechanical properties), and chemical properties (chemical structures, chemical composition) of wood were investigated by using scanning electron microscopy, confocal laser scanning microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, and dynamic vapor sorption. Meanwhile, the correlation between the mass changes and the color change, volumetric shrinkage, and hygroscopicity was also investigated. The results showed that the thermal degradation of wood cell wall components was the most important factor contributing to the changes in heat-induced shrinkage, color, and moisture adsorption of wood. In air-heat-treated wood samples, there was a significant correlation between mass change and heat-induced shrinkage, brightness, and moisture adsorption. However, the presence of impregnated tung oil in oil-heat-treated wood appears to disrupt these correlations among physical properties. The results of micromechanical properties demonstrated a significant decrease in elastic modulus following high-temperature heat treatment, which was mitigated by tung oil treatment. Chemical structure and compositional analyses indicated that the changes in chemical structure primarily stem from the degradation of hemicellulose and cellulose, and the presence of tung oil created an oxygen-insulating environment that slowed down this degradation process. Morphological observation results showed that tung oil permeated the wood structure and penetrated the cell walls through transportation channels, altering the micro-morphology of the cell wall surface, obstructing primary water passages (e.g., vessels and pits), and impeding the release of volatile degradation products as well as the infiltration and diffusion of water. In summary, tung oil treatment represents an environmentally friendly and efficient method for maximizing wood recovery and increasing product value. This approach holds significant potential for industrial applications in wood heat treatment.

Keywords: tung oil, heat treatment, physicochemical properties, wood cell walls

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Authors: Zahra Khan

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Hydrogels are a macromolecular network of hydrophilic copolymers with physical or chemical cross-linking structures with significant water uptake capabilities. They are a promising substrate for surface-enhanced Raman spectroscopy (SERS) as they are both flexible and biocompatible materials. Conventional SERS-active substrates suffer from limitations such as instability and inflexibility, which restricts their use in broader applications. Gelatin-based hydrogels have been synthesised in a facile and relatively quick method without the use of any toxic cross-linking agents. Composite gel material was formed by combining the gelatin with simple polymers to enhance the functional properties of the gel. Gold nanoparticles prepared by a reproducible seed-mediated growth method were combined into the bulk material during gel synthesis. After gel formation, the gel was submerged in the analyte solution overnight. SERS spectra were then collected from the gel using a standard Raman spectrometer. A wide range of analytes was successfully detected on these hydrogels showing potential for further optimization and use as SERS substrates for biomedical applications.

Keywords: gelatin, hydrogels, flexible materials, SERS

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Authors: Kun-Ting Song, Christian Schott, Peter Schneider, Sebastian Watzele, Regina Kluge, Elena Gubanova, Aliaksandr S. Bandarenka

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The combination of electrochemical impedance spectroscopy (EIS) and the hydrodynamic technique like rotation disc electrode (RDE) provides a critical method for quantitively investigating mechanisms of hydrogen evolution reaction (HER) in acidic and alkaline media. Pt5Gd represented higher HER activities than polycrystalline Pt (Pt(pc)) by means of the surface strain effects. The model of the equivalent electric circuit to fit the impedance data under the RDE configurations is developed. To investigate the relative reaction contribution, the ratio of the charge transfer reactions of the Volmer-Heyrovsky and Volmer-Tafel pathways on Pt and Pt5Gd electrodes is determined. The ratio remains comparably similar in acidic media, but it changes in alkaline media with Volmer–Heyrovsky pathway dominating. This combined approach of EIS and RDE can help to study the electrolyte effects and other essential reactions for electrocatalysis in future work.

Keywords: hydrogen evolution reaction, electrochemical impedance spectroscopy, hydrodynamic methods, electrocatalysis, electrochemical interface

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Authors: Bireswar Paul, Amitava Datta

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Indoor air environment is a big concern in the last few decades in the developing countries, with increased focus on monitoring the air quality. In this work, an experimental study has been conducted to establish the existence of carbon nanoparticles below the size range of 10 nm in the non-sooting zone of a LPG/air partially premixed flame. Mainly, four optical techniques, UV absorption spectroscopy, fluorescence spectroscopy, dynamic light scattering and TEM have been used to characterize and measure the size of carbon nanoparticles in the sampled materials collected from the inner surface of the flame front. The existence of the carbon nanoparticles in the sampled material has been confirmed with the typical nature of the absorption and fluorescence spectra already reported in the literature. The band gap energy shows that the particles are made up of three to six aromatic rings. The size measurement by DLS technique also shows that the particles below the size range of 10 nm. The results of DLS are also corroborated by the TEM image of the same material. 

Keywords: indoor air, carbon nanoparticle, lpg, partially premixed flame, optical techniques

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Authors: Cecilia Espindola, Juan Carlos Palacios

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Flavonoids are a large group of natural compounds which are found in many fruits and vegetables. A subgroup of these called flavanones display a wide range of biological activities, and they also have an important physiological role in plants. The ionic liquid (ILs) are compounds consisting of an organic cation with an organic or inorganic anion. Due to its unique properties such as high electrical conductivity, wide temperature range of the liquid state, thermal and electrochemical stability, high ionic density and low volatility and flammability, are considered as ecological solvents in organic synthesis, catalysis, electrolytes in accumulators, and electrochemistry, non-volatile plasticizers, and chemical separation. It was synthesized ionic liquid IL 1-butyl-3-methylimidazolium bromide free-solvent and used as reaction medium for flavanones synthesis, under several reaction conditions of temperature, time and production. The obtained compounds were analyzed by melting point, elemental analysis, IR and UV-vis spectroscopy.

Keywords: 1-butyl-3-methylimidazolium bromide, flavonoids, free-solvent, IR spectroscopy

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Authors: Osvaldo N. Oliveira Jr.

Abstract:

The control of molecular architecture inherent in some experimental methods to produce nanostructured films has had great impact on devices of various types, including sensors and biosensors. The self-assembly monolayers (SAMs) and the electrostatic layer-by-layer (LbL) techniques, for example, are now routinely used to produce tailored architectures for biosensing where biomolecules are immobilized with long-lasting preserved activity. Enzymes, antigens, antibodies, peptides and many other molecules serve as the molecular recognition elements for detecting an equally wide variety of analytes. The principles of detection are also varied, including electrochemical methods, fluorescence spectroscopy and impedance spectroscopy. In this presentation an overview will be provided of biosensors made with nanostructured films to detect antibodies associated with tropical diseases and HIV, in addition to detection of analytes of medical interest such as cholesterol and triglycerides. Because large amounts of data are generated in the biosensing experiments, use has been made of computational and statistical methods to optimize performance. Multidimensional projection techniques such as Sammon´s mapping have been shown more efficient than traditional multivariate statistical analysis in identifying small concentrations of anti-HIV antibodies and for distinguishing between blood serum samples of animals infected with two tropical diseases, namely Chagas´ disease and Leishmaniasis. Optimization of biosensing may include a combination of another information visualization method, the Parallel Coordinate technique, with artificial intelligence methods in order to identify the most suitable frequencies for reaching higher sensitivity using impedance spectroscopy. Also discussed will be the possible convergence of technologies, through which machine learning and other computational methods may be used to treat data from biosensors within an expert system for clinical diagnosis.

Keywords: clinical diagnosis, information visualization, nanostructured films, layer-by-layer technique

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Authors: G. C. Santini, C. Potrich, L. Lunelli, L. Vanzetti, S. Marasso, M. Cocuzza, C. Pederzolli

Abstract:

The relevance of circulating miRNAs as non-invasive biomarkers for several pathologies is nowadays undoubtedly clear, as they have been found to have both diagnostic and prognostic value able to add fundamental information to patients’ clinical picture. The availability of these data, however, relies on a time-consuming process spanning from the sample collection and processing to the data analysis. In light of this, strategies which are able to ease this procedure are in high demand and considerable effort have been made in developing Lab-on-a-chip (LOC) devices able to speed up and standardise the bench work. In this context, a very promising polydimethylsiloxane (PDMS)-based microdevice which integrates the processing of the biological sample, i.e. purification of extracellular miRNAs, and reverse transcription was previously developed in our lab. In this study, we aimed at the improvement of the miRNA extraction performances of this micro device by increasing the ability of its surface to absorb extracellular miRNAs from biological samples. For this purpose, we focused on the modulation of two properties of the material: roughness and charge. PDMS surface roughness was modulated by casting with several templates (terminated with silicon oxide coated by a thin anti-adhesion aluminum layer), followed by a panel of curing conditions. Atomic force microscopy (AFM) was employed to estimate changes at the nanometric scale. To introduce modifications in surface charge we functionalized PDMS with different mixes of positively charged 3-aminopropyltrimethoxysilanes (APTMS) and neutral poly(ethylene glycol) silane (PEG). The surface chemical composition was characterized by X-ray photoelectron spectroscopy (XPS) and the number of exposed primary amines was quantified with the reagent sulfosuccinimidyl-4-o-(4,4-dimethoxytrityl) butyrate (s-SDTB). As our final end point, the adsorption rate of all these different conditions was assessed by fluorescence microscopy by incubating a synthetic fluorescently-labeled miRNA. Our preliminary analysis identified casting on thermally grown silicon oxide, followed by a curing step at 85°C for 1 hour, as the most efficient technique to obtain a PDMS surface roughness in the nanometric scaleable to trap miRNA. In addition, functionalisation with 0.1% APTMS and 0.9% PEG was found to be a necessary step to significantly increase the amount of microRNA adsorbed on the surface, therefore, available for further steps as on-chip reverse transcription. These findings show a substantial improvement in the extraction efficiency of our PDMS microdevice, ultimately leading to an important step forward in the development of an innovative, easy-to-use and integrated system for the direct purification of less abundant circulating microRNAs.

Keywords: circulating miRNAs, diagnostics, Lab-on-a-chip, polydimethylsiloxane (PDMS)

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Authors: Manal Alhazmi, Artem Mishchenko

Abstract:

A molecular fluids' behavior and interaction with other materials at the nanoscale is a complex process. Nanoscale fluids behave so differently than macroscale fluids and interact with other materials in unique ways. It is, therefore, feasible to understand the molecular behavior of H₂O in such two-dimensional nanoscale systems by studying (CaSO4-2H2O), commonly known as gypsum. In the present study, spectroscopic measurements on a 2D structure of exfoliated gypsum crystals are carried out by Raman and IR spectroscopy. An array of gypsum flakes with thicknesses ranging from 8nm to 100nm were observed and analyzed for their Raman and IR spectrum. Water molecules stretching modes spectra lines were also measured and observed in nanoscale gypsum flakes and compared with those of bulk crystals. CaSO4-2H2O crystals have Raman and infrared bands at 3341 cm-1 resulting from the weak hydrogen bonds between the water molecules. This internal vibration of water molecules, together with external vibrations with other atoms, are responsible for these bands. There is a shift of about 70 cm-1 In the peak position of thin flakes with respect to the bulk crystal, which is a result of the different atomic arrangement from bulk to thin flake on the nano scale. An additional peak was observed in Raman spectra around 2910-3137 cm⁻¹ in thin flakes but is missing in bulk crystal. This additional peak is attributed to a combined mode of water internal (stretching mode at 3394cm⁻¹) and external vibrations. In addition to Raman and infra- red analysis of gypsum 2D structure, electrical measurements were conducted to reveal the water molecules transport behavior in such systems. Electrical capacitance of the fabricated device is measured and found to be (0.0686 *10-12) F, and the calculated dielectric constant (ε) is (12.26).

Keywords: gypsum, infra-red spectroscopy, raman spectroscopy, H₂O behavior

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Authors: P. Kumar, D. Eisenhauer, M. M. K. Yousef, Q. Shi, A. S. G. Khalil, M. R. Saber, C. Becker, T. Pullerits, K. J. Karki

Abstract:

In impedance spectroscopy (IS) the response of a photo-active device is analysed as a function of ac bias. It is widely applied in a broad class of material systems and devices. It gives access to fundamental mechanisms of operation of solar cells. We have implemented a method of IS where we modulate the light instead of the bias. This scheme allows us to analyze not only carrier dynamics but also impedance of device locally. Here, using this scheme, we have measured the frequency-dependent photocurrent response of the thin-film planar and nano-textured Si solar cells using this method. Photocurrent response is measured in range of 50 Hz to 50 kHz. Bode and Nyquist plots are used to determine characteristic lifetime of both the cells. Interestingly, the carrier lifetime of both planar and nano-textured solar cells depend on back and front contact positions. This is due to either heterogeneity of device or contacts are not optimized. The estimated average lifetime is found to be shorter for the nano-textured cell, which could be due to the influence of the textured interface on the carrier relaxation dynamics.

Keywords: carrier lifetime, impedance, nano-textured, photocurrent

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Authors: Mohammad Beyki, Justus Pawlak, Robert Patzke, Franz Renz

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In the context of planetary exploration, the MIMOS II (miniaturized Mössbauer spectrometer) serves as a proven and reliable measuring instrument. The transmission behaviour of the electronics in the Mössbauer spectroscopy is newly developed and optimized. For this purpose, the overall electronics is split into three parts. This elaboration deals exclusively with the first part of the signal chain for the evaluation of photons in experiments with gamma radiation. Parallel to the analysis of the electronics, a new method for the stability consideration of linear and non-linear systems is presented: The extended method of Lyapunov’s stability criteria. The design helps to weigh advantages and disadvantages against other simulated circuits in order to optimize the MIMOS II for the terestric and extraterestric measurment. Finally, after stability analysis, the controller design according to Ackermann is performed, achieving the best possible optimization of the output variable through a skillful pole assignment.

Keywords: Mössbauer spectroscopy, electronic signal amplifier, light processing technology, photocurrent, trans-impedance amplifier, extended Lyapunov method

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Authors: Takashi Kaburagi, Takamasa Komura, Yosuke Kurihara

Abstract:

Absolute pitch is the ability to identify a musical note without a reference tone. Training for absolute pitch often occurs in preschool education. It is necessary to clarify how well the trainee can make use of synesthesia in order to evaluate the effect of the training. To the best of our knowledge, there are no existing methods for objectively confirming whether the subject is using synesthesia. Therefore, in this study, we present a method to distinguish the use of color-auditory synesthesia from the separate use of color and audition during absolute pitch training. This method measures blood volume in the prefrontal cortex using functional Near-infrared spectroscopy (fNIRS) and assumes that the cognitive step has two parts, a non-linear step and a linear step. For the linear step, we assume a second order ordinary differential equation. For the non-linear part, it is extremely difficult, if not impossible, to create an inverse filter of such a complex system as the brain. Therefore, we apply a method based on a self-organizing map (SOM) and are guided by the available data. The presented method was tested using 15 subjects, and the estimation accuracy is reported.

Keywords: absolute pitch, functional near-infrared spectroscopy, prefrontal cortex, synesthesia

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Authors: Sarmistha Baruah, Akshai Kumar, Nageswara Rao Peela

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The global energy crisis due to the dependence on fossil fuels and its limited reserves as well as environmental pollution are key concerns to the research communities. However, the implementation of alcohol-based fuel cells such as methanol is anticipated as a reliable source of future energy technology due to their high energy density, environment friendliness, ease of storage, transportation, etc. To drive the anodic methanol oxidation reaction (MOR) in direct methanol fuel cells (DMFCs), an active and long-lasting catalyst is necessary for efficient energy conversion from methanol. Recently, transition metal-zeolite-based materials have been considered versatile catalysts for a variety of industrial and lab-scale processes. Large specific surface area, well-organized micropores, and adjustable acidity/basicity are characteristics of zeolites that make them excellent supports for immobilizing small-sized and highly dispersed metal species. Significant advancement in the production and characterization of well-defined metal clusters encapsulated within zeolite matrix has substantially expanded the library of materials available, and consequently, their catalytic efficacy. In this context, we developed bimetallic Ni-Co catalysts encapsulated within LTA (also known as 4A) zeolite via a method combined with the in-situ encapsulation of metal species using hydrothermal treatment followed by a chemical reduction process. The prepared catalyst was characterized using advanced characterization techniques, such as X-ray diffraction (XRD), field emission transmission electron microscope (FETEM), field emission scanning electron microscope (FESEM), energy dispersive X-ray (EDX), and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of the catalyst for MOR was carried out in an alkaline medium at room temperature using techniques such as cyclic voltammetry (CV), and chronoamperometry (CA). The resulting catalyst exhibited better catalytic activity of 12.1 mA cm-2 at 1.12 V vs Ag/AgCl and retained remarkable stability (~77%) even after 1000 cycles CV test for the electro-oxidation of methanol in alkaline media without any significant microstructural changes. The high surface area, better Ni-Co species integration in the zeolite, and the ample amount of surface hydroxyl groups contribute to highly dispersed active sites and quick analyte diffusion, which provide notable MOR kinetics. Thus, this study will open up new possibilities to develop a noble metal-free zeolite-based electrocatalyst due to its simple synthesis steps, large-scale fabrication, improved stability, and efficient activity for DMFC application.

Keywords: alkaline media, bimetallic, encapsulation, methanol oxidation reaction, LTA zeolite.

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Authors: Sudkate Chaiyo, Weena Siangproh, Orawon Chailapakul, Kurt Kalcher

Abstract:

In the present work, a simple and sensitive non-enzymatic electrochemical detection of glucose in disposable paper-based sensor was developed at ionic liquid/graphene/cobalt phthalocyanine composite (IL/G/CoPc) modified electrode. The morphology of the fabricated composite was characterized and confirmed by scanning electron microscopy and UV-Vis spectroscopy. The UV-Vis spectroscopy results confirmed that the G/CoPc composite formed via the strong π–π interaction between CoPc and G. Amperometric i-t technique was used for the determination of glucose. The response of glucose was linear over the concentration ranging from 10 µM to 1.5 mM. The response time of the sensor was found as 30 s with a limit of detection of 0.64 µM (S/N=3). The fabricated sensor also exhibited its good selectivity in the presence of common interfering species. In addition, the fabricated sensor exhibited its special advantages such as low working potential, good sensitivity along with good repeatability and reproducibility for the determination of glucose.

Keywords: glucose, paper-based sensor, ionic liquid/graphene/cobalt phthalocyanine composite, electrochemical detection

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