Search results for: photoacoustic spectroscopy

Authors: Kwame Sarkodie, William Cheung, Andrew R. Fergursson

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The characterization of multiphase flow has gained enormous attention for most petroleum and chemical industrial processes. In order to fully characterize fluid phases in a stream or containment, there needs to be a profound knowledge of the existing composition of fluids present. This introduces a problem for real-time monitoring of fluid dynamics such as fluid distributions, and phase fractions. This work presents a simple technique of correlating absorbance spectrums of water, oil and air bubble present in containment. These spectra absorption outputs are derived by using an Fourier Infrared spectrometer. During the testing, air bubbles were introduced into static water column and oil containment and with light absorbed in the infrared regions of specific wavelength ranges. Attenuation coefficients are derived for various combinations of water, gas and oil which reveal the presence of each phase in the samples. The results from this work are preliminary and viewed as a build up to the design of a multiphase flow rig which has an infrared sensor pair to be used for multiphase flow characterization.

Keywords: attenuation, infrared, multiphase, spectroscopy

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Authors: Jibon Sharma, Alakjyoti Patowary, Moirangthem Nara Singh

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In experimental research it is very much essential to obtain the quality control of the system used for the experiment. NaI (Tl) scintillation detector is the most commonly used in radiation and medical physics for measurement of the gamma ray activity of various samples. In addition, the scintillation detector has a lot of applications in the elemental analysis of various compounds, alloys using activation analysis. In each application for quantitative analysis, it is very much essential to know the detection efficiency and resolution for different gamma energies. In this work, the energy dependence of efficiency and resolution of NaI (Tl) detector using gamma-ray spectroscopy are investigated. Different photon energies of 356.01 keV,511keV,661.60keV,1170 keV,1274.53 keV and 1330 keV are obtained from four radioactive sources (133Ba,22Na,137Cs and 60 Co) used in these studies. Values of full energy peak efficiencies of these gamma energies are found to be respectively 58.46%,10.15%,14.39%,1.4%,3.27% and 1.31%. The values of percent resolution for above different gamma ray energies are found to be 11.27%,7.27%,6.38%,5.17%,4.86% and 4.74% respectively. It was found that the efficiency of the detector exponentially decreases with energy and the resolution of the detector is directly proportional to the energy of gamma-ray.

Keywords: naI (Tl) gamma-ray spectrometer, resolution, full energy peak efficiency, radioactive sources

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Authors: Kamel Taıbı, Abdelmadjid Rais

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Nickel–Aluminium ferrites with the general formula Ni Alx Fe2-x O4 (0 ≤ x ≤ 1) were studied using X-ray diffraction, Infra Red and Raman spectroscopy. XRD diffraction patterns and their Reitveld refinements show that all samples have a pure single-phase cubic spinel structure. From these patterns, the lattice parameters of these samples have been calculated and compared with those predicted theoretically. Most of the values were found to decrease with increasing Al content. Infra Red spectra showed two significant absorption bands. The high band corresponds to tetrahedral (A) sites and the lower band to octahedral [B] sites, thus confirming the single phase spinel structure. For all compositions, Raman spectra show the five active modes A1g + E1g + 3 T2g of the motion of O2- ions and both the A-site and B-site ions. The Raman frequencies trend with aluminium concentration show a blue shift for all modes consistent with the replacement of Fe3+ by lower mass Al3+. Composition dependence of the Raman frequency modes is discussed in relationship with the cations distribution among the A-sites and B-sites.

Keywords: Ni-Al ferrites, spinel structure, XRD, Raman spectroscopy

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Authors: M. D. Fontana, I. Bejaoui Ouni, D. Chapron, H. Aroui

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BaTiO3 (BT) is a well known ferroelectric material which has been thoroughly studied during several decades since it undergoes successive cubic-tetragonal-orthorhombic-rhombohedral phase transitions on cooling. It has several ferroelectric properties that allow it to be a good material for electronic applications such as the design of ferroelectric memories and pyroelectric elements. In the present work, we report the analysis of temperature dependence of Raman frequency and damping of the A1 modes polarized along the FE c axis as well as the optical phonons E corresponding to the ionic motions in the plane normal to c. Measurements were carried out at different temperatures ranging from 298 to 408 K (tetragonal phase) within different scattering configurations. Spectroscopic parameters of BT have determined using a high resolution Raman spectrometer and a fitting program. All the first order frequency modes exhibit a quasi linear decrease as function of the temperature, except for the A1[TO1], E[TO2] and E[TO4] lines which reveal a parabolic dependence illustrating an anharmonic process. The phonon frequency downshifts and damping evolutions are interpreted in terms of normal volume expansion and third- and fourth-order anharmonic potentials.

Keywords: BaTiO3, Raman spectroscopy, frequency, damping, anharmonic potential

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Authors: Pawel Albrycht, Monika Ksiezopolska-Gocalska, Robert Holyst

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Surface Enhanced Raman Spectroscopy (SERS) is a technique of growing importance not only in purely scientific research related to analytical chemistry. It finds more and more applications in broadly understood testing - medical, forensic, pharmaceutical, food - and everywhere works perfectly, on one condition that SERS substrates used for testing give adequate enhancement, repeatability, and homogeneity of SERS signal. This is a problem that has existed since the invention of this technique. Some laboratories use as SERS amplifiers colloids with silver or gold nanoparticles, others form rough silver or gold surfaces, but results are generally either weak or unrepeatable. Furthermore, these structures are very often highly specific - they amplify the signal only of a small group of compounds. It means that they work with some kinds of analytes but only with those which were used at a developer’s laboratory. When it comes to research on different compounds, completely new SERS 'substrates' are required. That underlay our decision to develop universal substrates for the SERS spectroscopy. Generally, each compound has different affinity for both silver and gold, which have the best SERS properties, and that's what depends on what signal we get in the SERS spectrum. Our task was to create the platform that gives a characteristic 'fingerprint' of the largest number of compounds with very high repeatability - even at the expense of the intensity of the enhancement factor (EF) (possibility to repeat research results is of the uttermost importance). As specified above SERS substrates are offered by SERSitive company. Applied method is based on cyclic potentiodynamic electrodeposition of silver or silver-gold nanoparticles on the conductive surface of ITO-coated glass at controlled temperature of the reaction solution. Silver nanoparticles are supplied in the form of silver nitrate (AgNO₃, 10 mM), gold nanoparticles are derived from tetrachloroauric acid (10 mM) while sodium sulfite (Na₂O₃, 5 mM) is used as a reductor. To limit and standardize the size of the SERS surface on which nanoparticles are deposited, photolithography is used. We secure the desired ITO-coated glass surface, and then etch the unprotected ITO layer which prevents nanoparticles from settling at these sites. On the prepared surface, we carry out the process described above, obtaining SERS surface with nanoparticles of sizes 50-400 nm. The SERSitive platforms present highly sensitivity (EF = 10⁵-10⁶), homogeneity and repeatability (70-80%).

Keywords: electrodeposition, nanoparticles, Raman spectroscopy, SERS, SERSitive, SERS platforms, SERS substrates

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Authors: Ouafek Nora, Keghouche Nassira, Dehdouh Heider, Untidt Carlos

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A lot of knowledge has been accumulated on the metal clusters supported on oxide surfaces because of their multiple applications in microelectronics, heterogeneous catalysis, and magnetic devices. In this work, the surface state of Ni / MgO has been studied by XPS (X-ray Photoemission Spectroscopy). The samples were prepared by impregnation with ion exchange Ni²⁺ / MgO, followed by either a thermal treatment in air (T = 100 -350 ° C) or a gamma irradiation (dose 100 kGy, 25 kGy dose rate h -1). The obtained samples are named after impregnation NMI, NMR after irradiation, and finally NMC(T) after calcination at the temperature T (T = 100-600 °C). A structural study by XRD and HRTEM reveals the presence of nanoscaled Ni-Mg intermetallic phases (Mg₂Ni, MgNi₂, and Mg₆Ni) and magnesium hydroxide. Mg(OH)₂ in nanometric range (2- 4 nm). Mg-Ni compounds are of great interest in energy fields (hydrogen storage…). XPS spectra show two Ni2p peaks at energies of about 856.1 and 861.9 eV, indicating that the nickel is primarily in an oxidized state on the surface. The shift of the main peak relative to the pure NiO (856.1 instead of 854.0 eV) suggests that in addition to oxygen, nickel is engaged in another link with magnesium. This is in agreement with the O1s spectra which present an overlap of peaks corresponds to NiO and MgO, at a calcination temperature T ≤ 300 °C.

Keywords: XPS, XRD, nanoparticules, Ni-MgO

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Pachari Chuenta, Suwat Nanan

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ZnO nanostructures have been synthesized successfully in high yield via catalyst-free chemical precipitation technique by varying zinc source (either zinc nitrate or zinc acetate) and oxygen source (either oxalic acid or urea) without using any surfactant, organic solvent or capping agent. The ZnO nanostructures were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), UV-vis diffuse reflection spectroscopy (UV-vis DRS), and photoluminescence spectroscopy (PL). The FTIR peak in the range of 450-470 cm-1 corresponded to Zn-O stretching in ZnO structure. The synthesized ZnO samples showed well crystalized hexagonal wurtzite structure. SEM micrographs displayed spherical droplet of about 50-100 nm. The band gap of prepared ZnO was found to be 3.4-3.5 eV. The presence of PL peak at 468 nm was attributed to surface defect state. The photocatalytic activity of ZnO was studied by monitoring the photodegradation of reactive red (RR141) azo dye under ultraviolet (UV) light irradiation. Blank experiment was also separately carried out by irradiating the aqueous solution of the dye in absence of the photocatalyst. The initial concentration of the dye was fixed at 10 mgL-1. About 50 mg of ZnO photocatalyst was dispersed in 200 mL dye solution. The sample was collected at a regular time interval during the irradiation and then was analyzed after centrifugation. The concentration of the dye was determined by monitoring the absorbance at its maximum wavelength (λₘₐₓ) of 544 nm using UV-vis spectroscopic analysis technique. The sources of Zn and O played an important role on photocatalytic performance of the ZnO photocatalyst. ZnO nanoparticles which prepared by zinc acetate and oxalic acid at molar ratio of 1:1 showed high photocatalytic performance of about 97% toward photodegradation of reactive red azo dye (RR141) under UV light irradiation for only 60 min. This work demonstrates the promising potential of ZnO nanomaterials as photocatalysts for environmental remediation.

Keywords: azo dye, chemical precipitation, photocatalytic, ZnO

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Authors: Ajay Krishnamurthy, Mariyappan Mahesh Kumar, Sellamuthu Periyar Selvam

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Fruits are considered as functional foods due to the presence of various bioactive compounds available such as polyphenols, which are beneficial to health when consumed as part of our diet. The primary objective of this study was to analyze the various functional groups present in ethanolic extracts of Hylocereus undatus and Garcinia indica and also measure their antibacterial and antioxidant potential respectively thereby affirming its nutraceutical potential. To fulfill our objective, a Fourier - transform Infrared Spectroscopy (FTIR) was conducted for functional group analysis, Total Phenolic Content and DPPH free radical scavenging activity for measuring it anti-oxidant potential and agar-well diffusion assay for antibacterial potential. On careful observation and analysis of the spectrum it was found that both the fruit extracts contain similar compounds viz. Phenols, Alkanes, Alkenes, Aldehydes, Ketones, Carboxylic Acid and Amines. Total phenolic content of H.undatus and G.indica was estimated to be (26.85 ± 1.84 mg GAE/100g) and (32.84 ± 1.63 mg GAE/100g) respectively which corresponds to an inhibition of 84% and 81% respectively. H.undatus shows an inhibition of (3.4 ± 2.1mm) in gram-positive and (4.2 ± 2.24mm) in gram-negative organism on the other hand G.indica shows (2.1 ± 0.98mm) in gram-positive and (3.1 ± 1.44mm) in gram negative. The presence of such diverse compounds in the fruits helps us to understand the necessity for the inclusion of fruits in our daily diet and also helps the pharmaceutical industry in realizing the importance of exotic fruits as a potential nutraceutical.

Keywords: DPPH, fourier-transform infrared spectroscopy (FTIR), Hylocereus undatus, Garcinia indica

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Authors: R. Sharma, A. Sil, S. Ray

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Nanocomposites gel polymer electrolytes are gaining more and more attention among the researchers worldwide due to their possible applications in various electrochemical devices particularly in solid-state Li-ion batteries. In this work we have investigated the effect of nanofibers on the electrical properties of PVDF-HFP based gel electrolytes. The nanocomposites polymer electrolytes have been synthesized by solution casting technique with 10wt% of ZrO2. By analysis of impedance spectroscopy it has been demonstrated that the incorporation of ZrO2 into PVDF-HFP–(PC+DEC)–LiClO4 gel polymer electrolyte system significantly enhances the ionic conductivity of the electrolyte. The enhancement of ionic conductivity seems to be correlated with the fact that the dispersion of ZrO2 to PVDF-HFP prevents polymer chain reorganization due to the high aspect ratio of ZrO2, resulting in reduction in polymer crystallinity, which gives rise to an increase in ionic conductivity. The decrease of crystallinity of PVDF-HFP due the addition of ZrO2 has been confirmed by XRD. The interaction of ZrO2 with various constituents of polymer electrolytes has been studied by FTIR spectroscopy. TEM results show that the fillers (ZrO2) has distributed uniformly in the polymer electrolytes. Moreover, ZrO2 added gel polymer electrolytes offer better thermal stability as compared to that of ZrO2 free electrolytes as confirmed by TGA analysis.

Keywords: polymer electrolytes, ZrO2, ionic conductivity, FTIR

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Authors: Radka Sefcu, Vaclava Antuskova, Ivana Turkova

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

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

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Authors: 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: 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: Abebe Taye

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The interest in enhancing the performance of all-solid-state batteries featuring lithium metal anodes as a potential alternative to traditional lithium-ion batteries has prompted exploration into new avenues. A promising strategy involves transforming lithium-ion batteries into hybrid configurations by integrating lithium-ion and lithium-metal solid-state components. This study is focused on achieving stable lithium deposition and advancing the electrochemical capabilities of solid-state lithium hybrid batteries with anodes by incorporating mesocarbon microbeads (MCMBs) blended with silver nanoparticles. To achieve this, mesocarbon microbeads (MCMBs) blended with silver nanoparticles are coated on stainless-steel current collectors. These samples undergo a battery of analyses employing diverse techniques. Surface morphology is studied through scanning electron microscopy (SEM). The electrochemical behavior of the coated samples is evaluated in both half-cell and full-cell setups utilizing an argyrodite-type sulfide electrolyte. The stability of MCMBs in the electrolyte is assessed using electrochemical impedance spectroscopy (EIS). Additional insights into the composition are gleaned through X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). At an ultra-low N/P ratio of 0.26, stability is upheld for over 100 charge/discharge cycles in half-cells. When applied in a full-cell configuration, the hybrid anode preserves 60.1% of its capacity after 80 cycles at 0.3 C under a low N/P ratio of 0.45. In sharp contrast, the capacity retention of the cell using untreated MCMBs declines to 20.2% after a mere 60 cycles. The introduction of mesocarbon microbeads (MCMBs) combined with silver nanoparticles into the hybrid anode of solid-state lithium batteries substantially elevates their stability and electrochemical performance. This approach ensures consistent lithium deposition and removal, mitigating dendrite growth and the accumulation of inactive lithium. The findings from this investigation hold significant value in elevating the reversibility and energy density of lithium-ion batteries, thereby making noteworthy contributions to the advancement of more efficient energy storage systems.

Keywords: MCMB, lithium metal, hybrid anode, silver nanoparticle, cycling stability

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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: 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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