Search results for: LIPS spectroscopy

Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. The present work simulates the contact between the calandria tube and the liquid injection shutdown system (LISS) nozzle. The Calandria tube is the outer covering of the pressure tube. Water flows inside the pressure tube through fuel claddings which produces vibration in the pressure tube along with vibration in the calandria tube. Fretting wear takes place at the point of contact between the calandria tube and the LISS nozzle. Fretting tests were performed under different conditions, such as; varying fretting duration (i.e., 1 to 4 hours), varying frequency (i.e., 5 to 6.5 Hz), and varying amplitude (100 to 400 µm). The formation of the oxide layer was observed during the fretting wear test; as a result, the worn product. The worn surfaces were analyzed with scanning electron microscopy (SEM) to analyze the wear mechanism involved in the fretting test, and Energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy were used to confirm the presence of an oxide layer on the worn surface. The oxide layer becomes more uniform with fretting duration in case of water submerged condition as compared to dry contact condition. The oxide layer is deeply removed at high amplitude due to the change of wear mechanism from adhesion to abrasion, as confirmed by the presence of micro ploughing and micro cutting. Low amplitude fretting favors the formation of the tribo-oxide layer.

Keywords: tribo-oxide layer, wear, mechanically mixed layer, zircaloy

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Authors: Kumari Kajal, Muthu Kumar Sampath, Hare Ram Singh

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In this context, the formulation and characterization of collagen silver lipid nanoparticles (CSLNs) were studied for their capacity to serve as fillers/matrix materials used in cosmeceutical applications. The CSLNs were prepared following a series of studies, such as X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) coupled with energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy FT-IR; thermogravimetric analysis (TGA); and differential scanning calorimetry (DSC). The studies confirmed the structural integrity of nanoparticles, their cargo and thermal stability. The biological functionality of CSLNs was studied by carrying out in vitro & in vivo studies. The antibacterial effect, hemocompatibility and anti-inflammatory characteristics of these fibers were systematically investigated. The toxicological assays included oral toxicity in mice and aquatic life tests with the fish Danio rerio model. The morphology of the nanoparticles was confirmed using high-resolution transmission electron microscopy (HR-TEM). The report found that CSLNs had strong antimicrobial effects, unmatched hemocompatibility, and low or absent inflammatory reactions, which makes them perfect candidates for cosmeceutical applications. The toxicological evaluations evinced a good safety record without any significant adverse effects in both murine and Danio rerio models. This research reveals the efficient way of CSLNs to the efficacy and safety of dermaceuticals.

Keywords: collagen silver lipid nanoparticles (CSLNs), cosmeceuticals, antimicrobial activity, hemocompatibility, in vitro assessment, in vivo assessment.

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Authors: Mandlenkosi George Robert Mahlobo, Tumelo Seadira, Major Melusi Mabuza, Peter Apata Olubambi

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Cathodic protection (CP) has been widely considered a suitable technique for mitigating corrosion of buried metal structures. Plenty of efforts have been made in developing techniques, in particular non-destructive techniques, for monitoring and quantifying the effectiveness of CP to ensure the sustainability and performance of buried steel structures. The aim of this study was to investigate the evolution of the electrochemical processes at the steel/soil interface during the application of CP on steel in simulated soil. Carbon steel was subjected to electrochemical tests with NS4 solution used as simulated soil conditions for 4 days before applying CP for a further 11 days. A previously modified non-destructive voltammetry technique was applied before and after the application of CP to measure the corrosion rate. Electrochemical impedance spectroscopy (EIS), in combination with mathematical modeling through equivalent electric circuits, was applied to determine the electrochemical behavior at the steel/soil interface. The measured corrosion rate was found to have decreased from 410 µm/yr to 8 µm/yr between days 5 and 14 because of the applied CP. Equivalent electrical circuits were successfully constructed and used to adequately model the EIS results. The modeling of the obtained EIS results revealed the formation of corrosion products via a mixed activation-diffusion mechanism during the first 4 days, while the activation mechanism prevailed in the presence of CP, resulting in a protective film. The x-ray diffraction analysis confirmed the presence of corrosion products and the predominant protective film corresponding to the calcareous deposit.

Keywords: carbon steel, cathodic protection, NS4 solution, voltammetry, EIS

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Authors: A. Katsman, L. Bloch, Y. Etinger, Y. Kauffmann, B. Pokroy

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Various nanosized amorphous alumina thin films in the range of (2.4 - 63.1) nm were deposited onto amorphous carbon and amorphous Si3N4 membrane grids. Transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), X-ray photoelectron spectroscopy (XPS) and differential scanning calorimetry (DSC) techniques were used to probe the size effect on the short range order and the amorphous to crystalline phase transition temperature. It was found that the short-range order changes as a function of size: the fraction of tetrahedral Al sites is greater in thinner amorphous films. This result correlates with the change of amorphous alumina density with the film thickness demonstrated by the reflectivity experiments: the thinner amorphous films have the less density. These effects are discussed in terms of surface reconstruction of the amorphous alumina films. The average atomic binding energy in the thin film layer decreases with decease of the thickness, while the average O-Al interatomic distance increases. The reconstruction of amorphous alumina is induced by the surface reconstruction, and the short range order changes being dependent on the density. Decrease of the surface energy during reconstruction is the driving force of the alumina reconstruction (density change) followed by relaxation process (short range order change). The amorphous to crystalline phase transition temperature measured by DSC rises with the decrease in thickness from 997.6°C for 13.9 nm to 1020.4 °C for 2.7 nm thick. This effect was attributed to the different film densities: formation of nanovoids preceding and accompanying crystallization process influences the crystallization rate, and by these means, the temperature of crystallization peak.

Keywords: amorphous alumina, density, short range order, size effect

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Authors: Sina Alimohammadi, Mahnaz Banihashemi, Maryam Poursharif

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Demodex is a mandatory parasite of pilosebaceous. D. folliculorum lives as a single parasite or as a number of parasites in hair follicles, and D. brevis as a single parasite living in sebaceous glands. Transmission of Demodex from one person to another requires direct skin contact; it also has a greater density in the forehead, cheeks, nose, and nasolabial folds. Demodex can cause some clinical symptoms such as follicular pityriasis, rosacea-like demodicosis, postural folliculitis, papules, seborrheic dermatitis, blepharitis, dermatitis around the lips, and hyperpigmented spots. In this study, the prevalence of Demodex species in patients referred to the dermatology department of Sayad Shirazi Hospital Gorgan, Iran, in the years 2019-2020 was investigated. Material and Methods: The study population consisted of 242 samples taken from the people referred to the dermatology department of Sayad Shirazi Hospital during the years 2019-2020, which were sampled by adhesive tape. All of the participants completed the questionnaires. The samples were examined microscopically for the presence of Demodex. Results: Out of 242 participants, 67 (27.68%) were infected with Demodex. Most cases of infection were observed in the group of 21 to 30 years (28 people; 11.57%) and then in the group of 31 to 40 years (21 people; 8.67%). Also, in the group of people under 10 years and over 60 years, no positive cases (0%) of Demodex were observed in microscopic examinations. Out of 11 variables, there was a statistically significant difference in relation to the three variables of age (P = 0.000003), use of cleansing solutions (P = 0.002), and the presence of acne (P = 0.0013). Conclusion: According to the results of this study, it was found that the incidence of Demodex in one group of acne patients is higher than in others, which emphasizes the possible role of Demodex in the pathogenesis of acne. In this study, there was an inverse relationship between the incidence of Demodex and the use of skin cleansing solutions. Also, the prevalence of Demodex is higher in the group of 20-30 years, and its prevalence does not increase with age. Due to the possibility of drug resistance in the future, regular studies on genotyping and drug resistance are recommended.

Keywords: acne, demodex, mite, prevalence

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Authors: Nidal Dwaikat

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This work presents the development of alpha spectroscopy method with Solid-state nuclear track detectors using aluminum thin films. The resolution of this method is high, and it is able to discriminate between alpha particles at different incident energy. It can measure the exact number of alpha particles at specific energy without needing a calibration of alpha track diameter versus alpha energy. This method was tested by using Cf-252 alpha standard source at energies 5.11 Mev, 3.86 MeV and 2.7 MeV, which produced by the variation of detector -standard source distance. On front side, two detectors were covered with two Aluminum thin films and the third detector was kept uncovered. The thickness of Aluminum thin films was selected carefully (using SRIM 2013) such that one of the films will block the lower two alpha particles (3.86 MeV and 2.7 MeV) and the alpha particles at higher energy (5.11 Mev) can penetrate the film and reach the detector’s surface. The second thin film will block alpha particles at lower energy of 2.7 MeV and allow alpha particles at higher two energies (5.11 Mev and 3.86 MeV) to penetrate and produce tracks. For uncovered detector, alpha particles at three different energies can produce tracks on it. For quality assurance and accuracy, the detectors were mounted on thick enough copper substrates to block exposure from the backside. The tracks on the first detector are due to alpha particles at energy of 5.11 MeV. The difference between the tracks number on the first detector and the tracks number on the second detector is due to alpha particles at energy of 3.8 MeV. Finally, by subtracting the tracks number on the second detector from the tracks number on the third detector (uncovered), we can find the tracks number due to alpha particles at energy 2.7 MeV. After knowing the efficiency calibration factor, we can exactly calculate the activity of standard source.

Keywords: aluminium thin film, alpha particles, copper substrate, CR-39 detector

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Authors: Muhammad Shahzad Tufail, Iram Liaqat

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Silver nanoparticles (AgNPs) have wider biomedical applications due to their intensive antimicrobial activities. However, toxicity and side effects of nanomaterials like AgNPs is a subject of great controversy towards the further studies in this direction. In this study, biogenically synthesized AgNPs, previously characterized via ultraviolet (UV) visible spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR), were subjected to toxicity evaluation using mice model. Albino male mice (BALB/c) were administered with 50 mgkg-1, 100 mgkg-1 and 150 mgkg-1 of AgNPs, respectively, except for control for 30 days. Log-probit regression analysis was used to measure the dosage response to determine the median lethal dose (LD50). Exposure to AgNPs caused significant changes in the levels of serum AST (P ˂ 0.05) at the 100mgkg-1 and 150mgkg-1 of AgNPs exposure, while ALT and serum creatinine (P ˃ 0.05) levels remained normal. Histopathology of male albino mice liver and kidney was studied after 30 days experimental period. Results revealed that mice exposed to heavy dose (150 mgkg-1) of AgNPs showed cell distortion, necrosis and detachment of hepatocytes in the liver. Regarding kidney, at lower concentration, normal renal structure with normal glomeruli was observed. However, at higher concentration (150 mgkg-1), kidneys showed smooth surface and dark red colour with proliferation of podocytes. It can be concluded from present study that biologically synthesized AgNPs are small to be eliminated easily by kidney and therefore the liver and kidney did not show toxicity at low concentrations.

Keywords: silver nanoparticles, pseudomonas aeruginosa, male albino mice, toxicity assessment

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Authors: Leonardo C. Pacheco-Londoño, Nataly J Galan-Freyle, Lisandro Pacheco-Lugo, Antonio Acosta-Hoyos, Elkin Navarro, Gustavo Aroca-Martinez, Karin Rondón-Payares, Alberto C. Espinosa-Garavito, Samuel P. Hernández-Rivera

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At the Life Science Research Center at Simon Bolivar University, a primary focus is the diagnosis of various diseases, and the use of gold nanoparticles (Au-NPs) in diverse biomedical applications is continually expanding. In the present study, Au-NPs were employed as substrates for Surface-Enhanced Raman Spectroscopy (SERS) aimed at diagnosing kidney diseases arising from Lupus Nephritis (LN), preeclampsia (PC), and Hypertension (H). Discrimination models were developed for distinguishing patients with and without kidney diseases based on the SERS signals from urine samples by partial least squares-discriminant analysis (PLS-DA). A comparative study of the Raman signals across the three conditions was conducted, leading to the identification of potential metabolite signals. Model performance was assessed through cross-validation and external validation, determining parameters like sensitivity and specificity. Additionally, a secondary analysis was performed using machine learning (ML) models, wherein different ML algorithms were evaluated for their efficiency. Models’ validation was carried out using cross-validation and external validation, and other parameters were determined, such as sensitivity and specificity; the models showed average values of 0.9 for both parameters. Additionally, it is not possible to highlight this collaborative effort involved two university research centers and two healthcare institutions, ensuring ethical treatment and informed consent of patient samples.

Keywords: SERS, Raman, PLS-DA, kidney diseases

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Authors: Nazanin Sheibanian, Raffaella Sesana, Sedat Ozbilen

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In recent years, high-entropy alloys (HEAs) have attracted considerable attention due to their unique properties and potential applications. In this study, novel HEA coatings were prepared on Mg substrates using mechanically alloyed HEA powder feedstocks based on Al_(0.1-0.5)CoCrCuFeNi and MnCoCrCuFeNi multi-material systems. The coatings were deposited by the Cold Spray (CS) process using three different temperatures of the process gas (N2) (650°C, 750°C, and 850°C) to examine the effect of gas temperature on coating properties. In this study, Infrared Thermography (non-destructive) was examined as a possible quality control technique for HEA coatings applied to magnesium substrates. Active Thermography was employed to characterize coating properties using the thermal response of the coating. Various HEA chemical compositions and deposition temperatures have been investigated. As a part of this study, a comprehensive macro and microstructural analysis of Cold Spray (CS) HEA coatings has been conducted using macrophotography, optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM+EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microhardness tests, roughness measurements, and porosity assessments. These analyses provided insight into phase identification, microstructure characterization, deposition, particle deformation behavior, bonding mechanisms, and identifying a possible relationship between physical properties and thermal responses. Based on the figures and tables, it is evident that the Maximum Relative Radiance (∆RMax) of each sample differs depending on both the chemical composition of HEA and the temperature at which Cold Spray is applied.

Keywords: active thermography, coating, cold spray, high- entropy alloy, material characterization

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Authors: Amal A. Al-Kahlawy, Heba H. El-Maghrabi

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Due to the increasing need to environment protection in real time need to energize new materials are under extensive investigations. Between others, TiO2 nanotubes (TNTs) nanocomposite with iron oxide and silver carbonate, are promising alternatives as high-efficiency visible light photocatalyst due to their unique properties and their superior charge transport properties. Our efforts in this domain aim the construction of novel nanocomposite of TiO2NT/Fe2O3@Ag2CO3. The structure, surface morphology, chemical composition and optical properties were characterized by X-ray diffraction (XRD), Raman, Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and UV–vis diffuse reflectance spectroscopy (DRS). XRD results confirm the interaction of TiO2-NT with iron oxide. This novel nanocomposite shows remarkably enhanced performance for phenol compounds photodegradation. The experimental data shows a promising photocatalytic activity. In particular, a maximum value of 450 mg/g was removed within 60 min at solar light irradiation with degradation efficiency of 99.5%. The high photocatalytic activity of the nanocomposite is found to be related to the increased adsorption toward chemical species, enhanced light absorption and efficient charge separation and transfer. Finally, the designed TiO2NT/Fe2O3@Ag2CO3 nanocomposite has a great degree of sustainability and could has a potential application for the industrial treatment of wastewater containing toxic organic materials.

Keywords: nanocomposite, photocatalyst, solar energy, titanium dioxide nanotubes

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Authors: Indu Chauhan, Bhupendra S. Butola, Paritosh Mohanty

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It is very well known that properties of material changes as their size approach to nanoscale level due to the high surface area to volume ratio. However, in last few decades, a tenet ‘structure dictates function’ is quickly being adopted by researchers working with nanomaterials. The design and exploitation of nanoparticles with tailored shape and size has become one of the primary goals of materials science researchers to expose the properties of nanostructures. To date, various methods, including soft/hard template/surfactant assisted route hydrothermal reaction, seed mediated growth method, capping molecule-assisted synthesis, polyol process, etc. have been adopted to synthesize the nanostructures with controlled size and shape and monodispersity. However controlling the shape and size of nanoparticles is an ultimate challenge of modern material research. In particular, many efforts have been devoted to rational and skillful control of hierarchical and complex nanostructures. Thus in our research work, role of cellulose in manipulating the nanostructures has been discussed. Nanoparticles of α-Fe₂O₃ (diameter ca. 15 to 130 nm) were immobilized on the cellulose fiber surface by a single step in situ hydrothermal method. However, nanoflakes of α-FeOOH having thickness ca. ~25 nm and length ca. ~250 nm were obtained by the same method in absence of cellulose fibers. A possible nucleation and growth mechanism of the formation of nanostructures on cellulose fibers have been proposed. The covalent bond formation between the cellulose fibers and nanostructures has been discussed with supporting evidence from the spectroscopic and other analytical studies such as Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The role of cellulose in manipulating the nanostructures has been discussed.

Keywords: cellulose fibers, α-Fe₂O₃, α-FeOOH, hydrothermal, nanoflakes, nanoparticles

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Authors: Mingqian Zhang

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Tip-enhanced Raman spectroscopy (TERS) is a scanning probe technique for individual objects and structured surfaces investigation that provides a wealth of enhanced spectral information with nanoscale spatial resolution and high detection sensitivity. It has become a powerful and promising chemical and physical information detection method in the nanometer scale. The TERS technique uses a sharp metallic tip regulated in the near-field of a sample surface, which is illuminated with a certain incident beam meeting the excitation conditions of the wave-vector matching. The local electric field, and, consequently, the Raman scattering, from the sample in the vicinity of the tip apex are both greatly tip-enhanced owning to the excitation of localized surface plasmons and the lightning-rod effect. Typically, a TERS setup is composed of a scanning probe microscope, excitation and collection optical configurations, and a Raman spectroscope. In the illumination configuration, an objective lens or a parabolic mirror is always used as the most important component, in order to focus the incident beam on the tip apex for excitation. In this research, a novel TERS setup was built up by introducing a plasmonic lens to the excitation optics as a focusing device. A plasmonic lens with symmetry breaking semi-annular slits corrugated on gold film was designed for the purpose of generating concentrated sub-wavelength light spots with strong longitudinal electric field. Compared to conventional far-field optical components, the designed plasmonic lens not only focuses an incident beam to a sub-wavelength light spot, but also realizes a strong z-component that dominants the electric field illumination, which is ideal for the excitation of tip-enhancement. Therefore, using a PL in the illumination configuration of TERS contributes to improve the detection sensitivity by both reducing the far-field background and effectively exciting the localized electric field enhancement. The FDTD method was employed to investigate the optical near-field distribution resulting from the light-nanostructure interaction. And the optical field distribution was characterized using an scattering-type scanning near-field optical microscope to demonstrate the focusing performance of the lens. The experimental result is in agreement with the theoretically calculated one. It verifies the focusing performance of the plasmonic lens. The optical field distribution shows a bright elliptic spot in the lens center and several arc-like side-lobes on both sides. After the focusing performance was experimentally verified, the designed plasmonic lens was used as a focusing component in the excitation configuration of TERS setup to concentrate incident energy and generate a longitudinal optical field. A collimated linearly polarized laser beam, with along x-axis polarization, was incident from the bottom glass side on the plasmonic lens. The incident light focused by the plasmonic lens interacted with the silver-coated tip apex and enhanced the Raman signal of the sample locally. The scattered Raman signal was gathered by a parabolic mirror and detected with a Raman spectroscopy. Then, the plasmonic lens based setup was employed to investigate carbon nanotubes and TERS experiment was performed. Experimental results indicate that the Raman signal is considerably enhanced which proves that the novel TERS configuration is feasible and promising.

Keywords: longitudinal electric field, plasmonics, raman spectroscopy, tip-enhancement

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Authors: Kaarour Abdelkrim, Ouardi Okkacha, Meskine Mohamed

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In this study, the υ_4 fundamental band of 12CD4 molecule has been studied by infrared spectroscopy with high resolution. Using XTDS and SPEVIEW software and the tensor formalism developed by ICB (laboratoire interdisciplinaire de Bourgogne) to several lines have been assigned and fitted with a standard deviation acceptable. This analysis allowed us to calculate several parameters of the molecule 12 CD4.

Keywords: XTDS, SPEVIEW, tetrahedral tensorial formalism, rovibrational band

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Authors: Malalage Mudara Peiris

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Objectives of the study are: the biosynthesis of silver nanoparticles (AgNPs) using Escherichia coli, Acinetobacter baumannii and Staphylococcus aureus, characterization of silver nanoparticles and determination of antimicrobial activity against E. coli, P. aeruginosa, S. aureus, MRSA, and C. Albicans. Methods: E. coli (ATCC 25922), A. baumanii (clinical strain), S. aureus (clinical strain) cultured in nutrient broth medium were used for biosynthesis of AgNPs. Culture conditions (AgNO3 concentration, pH, incubation time and temperature) were optimized. Characterization of synthesized NPs was done by UV-Visible spectroscopy. The antimicrobial activity of the synthesized NPs was studied using the good diffusion assay against E. coli, S. aureus, MRSA (Methicillin-resistant Staphylococcus aureus), P. aeruginosa and C. Albicans. Results: All the selected bacteria produced silver nanoparticles at alkaline pH above 0.3 g/L AgNO3 concentration. The optimum reaction temperature was 60oC. According to the UV-Visible spectroscopy, the maximum absorbance was found to be around 420 - 430 nm indicating the presence of AgNPs. According to the good diffusion results, AgNPs produced by S. aureus resulted in the larger zone of inhibition (ZOI) against the selected pathogens, while AgNPs produced by E. coli showed comparatively smaller ZOI. In general, biosynthesized AgNPs were highly effective against gram-negative bacteria compared to gram-positive bacterial and fungal species. Conclusions: Green AgNPs produced by each bacterium show antimicrobial activity against the selected pathogens. AgNPs produced by S. aureus are the most effective NPs among tested AgNPs, while AgNPs produced by E. coli are the least effective. Further characterization of NPs is required to study the physical properties of silver NPs.

Keywords: green nanotechnology, silver nanoparticles, bacteria, antimicrobial activity

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Authors: Singh Deepeshwar, Suhas Vinchurkar

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Similar to neuroimaging findings through functional magnetic resonance imaging (fMRI) assessing regional cerebral blood oxygenation, the functional near infrared spectroscopy (fNIRS) has also been used to assess hemodynamic responses in the imaged region of the brain. The present study assessed hemodynamic responses in terms of changes in oxygenation (HbO), deoxygenation (HbR) and total hemoglobin (THb) on the prefrontal cortex (PFC), bilaterally, using fNIRS in 10 participants who performed three voluntary regulated breathing (pranayama) practices viz. (i) Left nostril breathing (LNB), (ii) Right nostril breathing (RNB); and (iii) Alternating nostril breathing (ANB) and compared with normal breathing as baseline (BS). For this, we used 64 channel NIRS system covering left and the right prefrontal cortex. The normal breathing kept as baseline (BS) measures as regressors in the investigation of hemodynamic responses when compared with LNB, RNB and ANB. In the results, we found greater oxygenation in contralateral side i.e., higher activation on the left prefrontal cortex (lPFC) during RNB, and right prefrontal cortex (rPFC) during LNB, whereas ANB showed greater deoxygenation responses on both sides of PFC. Interestingly, LNB showed increased oxygenation on ipsilateral side i.e., lPFC but not during RNB. This suggests that voluntary regulated breathing produced an immediate effect not only on contralateral but ipsilateral sides of the brain as well. In conclusion, breathing practices are tightly coupled to cerebral rhythms of alternating cerebral hemispheric activity during particular nostril breathing. These results of the specific nostril breathing do not support previous findings of contralateral hemispheric improvement while left or right nostril breathing only.

Keywords: hemodynamic responses, brain, pranayama, voluntary regulated breathing practices, prefrontal cortex

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Authors: Beatriz Muñiz Cano, J. Ripoll Sau, D. Pacile, P. M. Sheverdyaeva, P. Moras, J. Camarero, R. Miranda, M. Garnica, M. A. Valbuena

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Graphene, in its pristine state, is a semiconductor with a zero band gap and massless Dirac fermions carriers, which conducts electrons like a metal. Nevertheless, the absence of a bandgap makes it impossible to control the material’s electrons, something that is essential to perform on-off switching operations in transistors. Therefore, it is necessary to generate a finite gap in the energy dispersion at the Dirac point. Intense research has been developed to engineer band gaps while preserving the exceptional properties of graphene, and different strategies have been proposed, among them, quantum confinement of 1D nanoribbons or the introduction of super periodic potential in graphene. Besides, in the context of developing new 2D materials and Van der Waals heterostructures, with new exciting emerging properties, as 2D transition metal chalcogenides monolayers, it is fundamental to know any possible interaction between chalcogenide atoms and graphene-supporting substrates. In this work, we report on a combined Scanning Tunneling Microscopy (STM), Low Energy Electron Diffraction (LEED), and Angle-Resolved Photoemission Spectroscopy (ARPES) study on a new superstructure when Te is evaporated (and intercalated) onto graphene over Ir(111). This new superstructure leads to the electronic doping of the Dirac cone while the linear dispersion of massless Dirac fermions is preserved. Very interestingly, our ARPES measurements evidence a large band gap (~400 meV) at the Dirac point of graphene Dirac cones below but close to the Fermi level. We have also observed signatures of the Dirac point binding energy being tuned (upwards or downwards) as a function of Te coverage.

Keywords: angle resolved photoemission spectroscopy, ARPES, graphene, spintronics, spin-orbitronics, 2D materials, transition metal dichalcogenides, TMDCs, TMDs, LEED, STM, quantum materials

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Authors: Nabil Al-Zaqri

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Semiconductor photocatalysts with surface defects display incredible light absorption bandwidth, and these defects function as highly active sites for oxidation processes by interacting with the surface band structure. Accordingly, engineering the photocatalyst with surface oxygen vacancies will enhance the semiconductor nanostructure's photocatalytic efficiency. Herein, a CeO2₋ₓ nanostructure is designed under the influence of low-frequency ultrasonic waves to create surface oxygen vacancies. This approach enhances the photocatalytic efficiency compared to many heterostructures while keeping the intrinsiccrystal structure intact. Ultrasonic waves induce the acoustic cavitation effect leading to the dissemination of active elements on the surface, which results in vacancy formation in conjunction with larger surface area and smaller particle size. The structural analysis of CeO₂₋ₓ revealed higher crystallinity, as well as morphological optimization, and the presence of oxygen vacancies is verified through Raman, X-rayphotoelectron spectroscopy, temperature-programmed reduction, photoluminescence, and electron spinresonance analyses. Oxygen vacancies accelerate the redox cycle between Ce₄+ and Ce₃+ by prolongingphotogenerated charge recombination. The ultrasound-treated pristine CeO₂ sample achieved excellenthydrogen production showing a quantum efficiency of 1.125% and efficient organic degradation. Ourpromising findings demonstrated that ultrasonic treatment causes the formation of surface oxygenvacancies and improves photocatalytic hydrogen evolution and pollution degradation. Conclusion: Defect engineering of the ceria nanoparticles with oxygen vacancies was achieved for the first time using low-frequency ultrasound treatment. The U-CeO₂₋ₓsample showed high crystallinity, and morphological changes were observed. Due to the acoustic cavitation effect, a larger surface area and small particle size were observed. The ultrasound treatment causes particle aggregation and surface defects leading to oxygen vacancy formation. The XPS, Raman spectroscopy, PL spectroscopy, and ESR results confirm the presence of oxygen vacancies. The ultrasound-treated sample was also examined for pollutant degradation, where 1O₂was found to be the major active species. Hence, the ultrasound treatment influences efficient photocatalysts for superior hydrogen evolution and an excellent photocatalytic degradation of contaminants. The prepared nanostructure showed excellent stability and recyclability. This work could pave the way for a unique post-synthesis strategy intended for efficient photocatalytic nanostructures.

Keywords: surface defect, CeO₂₋ₓ, photocatalytic, water treatment, H₂ production

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Authors: Bhairi Lakshminarayana, Surajit Sarker, Ch. Subrahmanyam

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The present study reports the development of noble metal free nano catalysts for low-temperature CO oxidation and water gas shift reaction. Mn-substituted CeO2 solid solution catalysts were synthesized by co-precipitation, combustion and hydrothermal methods. The formation of solid solution was confirmed by XRD with Rietveld refinement and the percentage of carbon and nitrogen doping was ensured by CHNS analyzer. Raman spectroscopic confirmed the oxygen vacancies. The surface area, pore volume and pore size distribution confirmed by N2 physisorption analysis, whereas, UV-visible diffuse reflectance spectroscopy and XPS data confirmed the oxidation state of the Mn ion. The particle size and morphology (spherical shape) of the material was confirmed using FESEM and HRTEM analysis. Ce0.8Mn0.2O2-δ was calcined at 400 °C, 600 °C and 800 °C. Raman spectroscopy confirmed that the catalyst calcined at 400 °C has the best redox properties. The activity of the designed catalysts for CO oxidation (0.2 vol%), carried out with GHSV of 21,000 h-1 and it has been observed that co-precipitation favored the best active catalyst towards CO oxidation and water gas shift reaction, due to the high surface area, improved reducibility, oxygen mobility and highest quantity of surface oxygen species. The activation energy of low temperature CO oxidation on Ce0.8Mn0.2O2- δ (combustion) was 5.5 kcal.K-1.mole-1. The designed catalysts were tested for water gas shift reaction. The present study demonstrates that Mn ion substituted ceria at 400 °C calcination temperature prepared by co-precipitation method promise to revive a green sustainable energy production approach.

Keywords: Ce0.8Mn0.2O2-ð, CO oxidation, physicochemical characterization, water gas shift reaction (WGS)

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Authors: Amit Keshav, Alok Sharma, Bidyut Mazumdar

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Colocasia esculenta leaves and roots are widely used in Asian countries, such as, India, Srilanka and Pakistan, as food and feed material. The root is high in carbohydrates and rich in zinc. The leaves and stalks are often traditionally preserved to be eaten in dry season. Leaf juice is stimulant, expectorant, astringent, appetizer, and otalgia. Looking at the medicinal uses of the plant leaves; phytochemicals were extracted from the plant leaves and were characterized using Fourier-transform infrared spectroscopy (FTIR) to find the functional groups. Phytochemical analysis of Colocasia esculenta (L.) leaf was studied using three solvents (methanol, chloroform, and ethanol) with soxhlet apparatus. Powder of the leaves was employed to obtain the extracts, which was qualitatively and quantitatively analyzed for phytochemical content using standard methods. Phytochemical constituents were abundant in the leave extract. Leaf was found to have various phytochemicals such as alkaloids, glycosides, flavonoids, terpenoids, saponins, oxalates and phenols etc., which could have lot of medicinal benefits such as reducing headache, treatment of congestive heart failure, prevent oxidative cell damage etc. These phytochemicals were identified using UV spectrophotometer and results were presented. In order to find the antioxidant activity of the extract, DPPH (2,2-diphenyl-1-picrylhydrazyl) method was employed using ascorbic acid as standard. DPPH scavenging activity of ascorbic acid was found to be 84%, whereas for ethanol it was observed to be 78.92%, for methanol: 76.46% and for chloroform: 72.46%. Looking at the high antioxidant activity, Colocasia esculenta may be recommended for medicinal applications. The characterizations of functional groups were analyzed using FTIR spectroscopy.

Keywords: antioxidant activity, Colocasia esculenta, leaves, characterization, FTIR

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Authors: Elizabeth O. Odewale, Sachithra T. Wanasinghe, Aaron S. Rury

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Cavity polaritons form when molecular excitons strongly couple to photons in carefully constructed optical cavities. These polaritons, which are hybrid light-matter states possessing a unique combination of photonic and excitonic properties, present the opportunity to manipulate the properties of various semiconductor materials. The systematic manipulation of materials through polariton formation could potentially improve the functionalities of many optoelectronic devices such as lasers, light-emitting diodes, photon-based quantum computers, and solar cells. However, the prospects of leveraging polariton formation for novel devices and device operation depend on more complete connections between the properties of molecular chromophores, and the hybrid light-matter states they form, which remains an outstanding scientific goal. Specifically, for most optoelectronic applications, it is paramount to understand how polariton formation affects the spectra of light absorbed by molecules coupled strongly to cavity photons. An essential feature of a polariton state is its dispersive energy, which occurs due to the enhanced spatial delocalization of the polaritons relative to bare molecules. To leverage the spatial delocalization of cavity polaritons, angle-resolved photoluminescence excitation spectroscopy was employed in characterizing light emission from the polaritonic states. Using lasers of appropriate energies, the polariton branches were resonantly excited to understand how molecular light absorption changes under different strong light-matter coupling conditions. Since an excited state has a finite lifetime, the photon absorbed by the polariton decays non-radiatively into lower-lying molecular states, from which radiative relaxation to the ground state occurs. The resulting fluorescence is collected across several angles of excitation incidence. By modeling the behavior of the light emission observed from the lower-lying molecular state and combining this result with the output of angle-resolved transmission measurements, inferences are drawn about how the behavior of molecules changes when they form polaritons. These results show how the intrinsic properties of molecules, such as the excitonic lifetime, affect the rate at which the polaritonic states relax. While it is true that the lifetime of the photon mediates the rate of relaxation in a cavity, the results from this study provide evidence that the lifetime of the molecular exciton also limits the rate of polariton relaxation.

Keywords: flourescece, molecules in cavityies, optical cavity, photoluminescence excitation, spectroscopy, strong coupling

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Authors: Ouahiba Bechiri, Mostefa Abbessi

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In recent year, polyoxometallates are intensely being explored because of their applications as new materiels, structural aesthetics, catalysts, and biologically active compounds. heteropolyanions of general formulae [X2M18O62] n- (X= heteroatom, e.g. P, Si) and (M=W, Mo), known as Dawson-type anions, constitue a special class of polyoxometallate compounds. In this present work, cobalt substituted heteropolyanion Dawson-type [HP2W15Mo3CoO61] were synthesized and characterized by IR spectroscopy, 31 P NMR, cyclic voltammetry.

Keywords: heteropolyanions, nanomaterials, Dawson-type, characterization

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Authors: Sharjeel Abid, Tanveer Hussain, Ahsan Nazir, Abdul Zahir, Nabyl Khenoussi

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Localized application of drug has various advantages and fewer side effects as compared with other methods. Burn patients suffer from swear pain and the major aspects that are considered for burn victims include pain and infection management. Nano-fibers (NFs) loaded with drug, applied on local wound area, can solve these problems. Therefore, this study dealt with the fabrication of drug loaded NFs for better pain management. Two layers of NFs were fabricated with different drugs. Contact layer was loaded with Gabapentin (a nerve painkiller) and the second layer with acetaminophen. The fabricated dressing was characterized using scanning electron microscope, Fourier Transform Infrared Spectroscopy, X-Ray Diffraction and UV-Vis Spectroscopy. The double layered based NFs dressing was designed to have both initial burst release followed by slow release to cope with pain for two days. The fabricated nanofibers showed diameter < 300 nm. The liquid absorption capacity of the NFs was also checked to deal with the exudate. The fabricated double layered dressing with dual drug loading and release showed promising results that could be used for dealing pain in burn victims. It was observed that by the addition of drug, the size of nanofibers was reduced, on the other hand, the crystallinity %age was increased, and liquid absorption decreased. The combination of fast nerve pain killer release followed by slow release of non-steroidal anti-inflammatory drug could be a good tool to reduce pain in a more secure manner with fewer side effects.

Keywords: pain management, burn wounds, nano-fibers, controlled drug release

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Authors: S. Singh, P. Patel, D. Kachhadiya, Swapnil Dharaskar

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The research objective is to integrate nanoparticles into fuels- i.e. diesel, biodiesel, biodiesel blended with diesel, plastic derived fuels, etc. to increase the fuel efficiency. The metal oxide nanoparticles will reduce the carbon monoxide emissions by donating oxygen atoms from their lattices to catalyze the combustion reactions and to aid complete combustion; due to this, there will be an increase in the calorific value of the blend (fuel + metal nanoparticles). Aluminium oxide and cobalt oxide nanoparticles have been synthesized by sol-gel method. The characterization was done by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscopy (EDS). The size of the particles was determined by XRD to be 28.6 nm and 28.06 nm for aluminium oxide and cobalt oxide nanoparticles respectively. Different concentration blends- 50, 100, 150 ppm were prepared by adding the required weight of metal oxides in 1 liter of diesel and sonicating for 30 minutes at 500W. The blend properties- calorific value, viscosity, and flash point were determined by bomb calorimeter, Brookfield viscometer and pensky-martin apparatus. For the aluminum oxide blended diesel, there was a maximum increase of 5.544% in the calorific value, but at the same time, there was an increase in the flash point from 43°C to 58.5°C and an increase in the viscosity from 2.45 cP to 3.25 cP. On the other hand, for the cobalt oxide blended diesel there was a maximum increase of 2.012% in the calorific value while the flash point increased from 43°C to 51.5°C and the viscosity increased from 2.45 cP to 2.94 cP. There was a linear increase in the calorific value, viscosity and flash point when the concentration of the metal oxide nanoparticles in the blend was increased. For the 50 ppm Al₂O₃ and 50 ppm Co₃O₄ blend the increasing the calorific value was 1.228 %, and the viscosity changed from 2.45 cP to 2.64 cP and the flash point increased from 43°C to 50.5°C. Clearly the aluminium oxide nanoparticles increase the calorific value but at the cost of flash point and viscosity, thus it is better to use the 50 ppm aluminium oxide, and 50 ppm cobalt oxide blended diesel.

Keywords: aluminium oxide nanoparticles, cobalt oxide nanoparticles, fuel additives, fuel characteristics

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Authors: Swapna N., Deepthy Ann Joy

Abstract:

One of the major causes of communication disorders in pediatric population is Motor speech disorders. These disorders which affect the motor aspects of speech articulators can have an adverse effect on the communication abilities of children in their developmental period. The motor aspects are dependent on the sensory abilities of children with motor speech disorders. Hence, oral sensorimotor evaluation is an important component in the assessment of children with motor speech disorders. To our knowledge, the importance of oral motor examination has been well established, yet the sensory assessment of the oral structures has received less focus. One of the most common motor speech disorders seen in children is developmental dysarthria. The present study aimed to assess the orosensory aspects in children with developmental dysarthria (CDD). The control group consisted of 240 children in the age range of four and eight years which was divided into four subgroups (4-4.11, 5-5.11, 6-6.11 and 7-7.11 years). The experimental group consisted of 15 children who were diagnosed with developmental dysarthria secondary to cerebral palsy who belonged in the age range of four and eight years. The oro-sensory aspects such as response to touch, temperature, taste, texture, and orofacial sensitivity were evaluated and profiled. For this purpose, the authors used the ‘Oral Sensorimotor Evaluation Protocol- Children’ which was developed by the authors. The oro-sensory section of the protocol was administered and the clinical profile of oro-sensory abilities of typically developing children and CDD was obtained for each of the sensory abilities. The oro-sensory abilities of speech articulators such as lips, tongue, palate, jaw, and cheeks were assessed in detail and scored. The results indicated that experimental group had poorer scores on oro-sensory aspects such as light static touch, kinetic touch, deep pressure, vibration and double simultaneous touch. However, it was also found that the experimental group performed similar to control group on few aspects like temperature, taste, texture and orofacial sensitivity. Apart from the oro-motor abilities which has received utmost interest, the variation in the oro-sensory abilities of experimental and control group is highlighted and discussed in the present study. This emphasizes the need for assessing the oro-sensory abilities in children with developmental dysarthria in addition to oro-motor abilities.

Keywords: cerebral palsy, developmental dysarthria, orosensory assessment, touch

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Authors: Saidasanov Saidazal Shokhmurodovich, Topolnickiy Orest Zinovyevich, Afaunova Olga Arturovna

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Relevance: Bilateral congenital cleft is one of the most complex forms of all clefts, which makes it difficult to choose a surgical method of treatment. During primary operations to close the hard and soft palate, there is a shortage of soft tissues and their lack during standard uranoplasty, and these factors aggravate the period of rehabilitation of patients. Materials and methods: The results of surgical treatment of children with bilateral cleft, who underwent uranoplasty using a flap from the tongue, were analyzed. The study used methods: clinical and statistical, which allowed us to solve the tasks, based on the principles of evidence-based medicine. Results and discussion: in our study, 15 patients were studied, who underwent surgical treatment in the following volume: uranoplasty using a flap from the tongue in two stages. Of these, 9 boys and 6 girls aged 2.5 to 6 years. The first stage was surgical treatment in the volume: veloplasty. The second stage was a surgical intervention in volume: uranoplasty using a flap from the tongue. In all patients, the width of the cleft ranged from 1.6-2.8 cm. All patients in this group were orthodontically prepared. Using this method, the surgeon can achieve the following results: maximum narrowing of the palatopharyngeal ring, long soft palate, complete closure of the hard palate, alveolar process, and the mucous membrane of the nasal cavity is also sutured, which creates good conditions for the next stage of osteoplastic surgery. Based on the result obtained, patients have positive results of working with a speech therapist. In all patients, the dynamics were positive without complications. Conclusions: Based on our observation, tongue flap uranoplasty is one of the effective techniques for patients with wide clefts of the hard and soft palate. The use of a flap from the tongue makes it possible to reduce the number of repeated reoperations and improve the quality of social adaptation of this group of patients, which is one of the important stages of rehabilitation. Upon completion of the stages of rehabilitation, all patients had the maximum improvement in functional, anatomical and social indicators.

Keywords: congenital cleft lips and palate, bilateral cleft, child surgery, maxillofacial surgery

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Authors: Fatai O. Oladoyinbo, Felix O. Sanni, Akinwunmi Fatai, Kamoli A. Amusa, Saheed A. Ganiyu, Wasiu B. Ayinde, Tajudeen A. Afolabi, Enock O. Dare

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Silver (Ag) and silica (SiO2) nanoparticles were synthesized using the chemical reduction method from silver nitrate and sodium silicate, respectively. X-ray Diffraction (XRD), High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), Uv-Visible spectroscopy, Energy Dispersive X-ray (EDX) spectroscopy and N2 adsorption-desorption techniques were utilized to characterize the composition and structure of the samples. The crystallinity pattern of Ag nanoparticles was indexed as (111), (200), (220) and (311), which allowed reflections from face-centered cubic silver. XRD of SiO2 showed good porosity with a broad-spectrum band at Bragg’s angle 2θ of 22° while that of Ag-SiO2 showed distinct peaks at 2θ values of 39°, 43°, 66° and 79°. The XRD result agreed perfectly with the SEM and HRTEM images which showed Ag-SiO2 isotropic and anisotropic under the varying concentration of reactants. The elemental composition of Ag-SiO2, as displayed by EDX, confirmed Ag enrichment in the Ag-SiO2 heterostructure. The Uv-Visible peak at 421 nm confirmed the Surface Plasmon Resonance absorption peak of silver nanoparticles. N2 adsorption-desorption result showed a broad band of Ag-SiO2 from 3 to 8 nm, which indicated relatively narrow pore size distributions. Humidity sensing measurements performed in a controlled humidity chamber showed very high sensitivity with a sensitivity factor (SF) of 4.63 and high linearity with a steady decrease in resistance to humidity from 880 Ω at 10% RH to 190 Ω at 100% RH, indicating that Ag-SiO2 nanocomposite is a good sensing material with high sensitivity and linearity.

Keywords: silver, silica, nanocomposite, synthesis, heterostructure, core shell

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Authors: Mamatha Hosapatna, Anne D. Souza, Vrinda Hari Ankolekar, Antony Sylvan D. Souza

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Introduction: The lower extremity of the femur is characterized by an anterior groove in which patella is held during motion. This groove separates the two lips of the trochlea (medial and lateral), prolongation of the two condyles. In humans, the lateral trochlear lip is more developed than the medial one, creating an asymmetric groove that is also specific to the human body. Because of femoral obliquity, contraction of quadriceps leads to a lateral dislocation stress on the patella, and the more elevated lateral side of the patellar groove helps the patella stays in its correct place, acting as a wall against lateral dislocation. This specific shape fits an oblique femur. It is known that femoral obliquity is not genetically determined but comes with orthostatism and biped walking. Material and Methodology: To measure the various dimensions of the Femoropatellar groove (FPG) and femoral condyle using digital image analyser. 37 dried adult femora (22 right,15 left) were used for the study. End on images of the lower end of the femur was taken. Various dimensions of the Femoropatellar groove and FP angle were measured using image J software. Results were analyzed statistically. Results: Maximum of the altitude of medial condyle of the right femur is 4.98± 0.35 cm and of the left femur is 5.20±.16 cm. Maximum altitude of lateral condyle is 5.44±0.4 and 5.50±0.14 on the right and left side respectively. Medial length of the groove is 1.30±0.38 cm on the right side and on the left side is 1.88±0.16 cm. The lateral length of the groove on the right side is 1.900±.16 cm and left side is 1.88±0.16 cm. Femoropatellar angle is 136.38◦±2.59 on the right side and on the left side it is 142.38◦±7.0 Angle and dimensions of the femoropatellar groove on the medial and lateral sides were measured. Asymmetry in the patellar groove was observed. The lateral lip was found to be wider and bigger which correlated with the previous studies. An asymmetrical patellar groove with a protruding lateral side associated with an oblique femur is a specific mark of bipedal locomotion. Conclusion: Dimensions of FPG are important in maintaining the stability of patella and also in knee replacement surgeries. The implants used in to replace the patellofemoral compartment consist of a metal groove to fit on the femoral end and a plastic disc that attaches to the undersurface of the patella. The location and configuration of the patellofemoral groove of the distal femur are clinically significant in the mechanics and pathomechanics of the patellofemoral articulation.

Keywords: femoral patellar groove, femoro patellar angle, lateral condyle, medial condyle

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Authors: Patricia Mikchaela D. L. Feliciano, Ciela Kadeshka A. Fuentes, Bea Trixia B. Gales, Ethel Princess A. Gepulango, Martin R. Hernandez, Elina Andrea S. Lantion, Jhoe Cynder P. Legaspi, Peter F. Quilala, Gina C. Castro

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Propolis is a resin-like material used by bees to fill large gap holes in the beehive. It has been found to possess anti-inflammatory property, which stimulates hair growth in rats by inducing hair keratinocytes proliferation, causing water retention and preventing damage caused by heat, ultraviolet rays, and other microorganisms without abnormalities in hair follicles. The present study aimed to formulate 10% and 30% Propolis Hair Cream for use in enhancing hair properties. Raw propolis sample was tested for heavy metals using Atomic Absorption Spectroscopy; zinc and chromium were found to be present. Likewise, propolis was extracted in a percolator using 70% ethanol and concentrated under vacuum using a rotary evaporator. The propolis extract was analyzed for total flavonoid content. Compatibility of the propolis extract with excipients was evaluated using Differential Scanning Calorimetry (DSC). No significant changes in organoleptic properties, pH and viscosity of the formulated creams were noted after four weeks of storage at 2-8°C, 30°C, and 40°C. The formulated creams were found to be non-irritating based on the Modified Draize Rabbit Test. In vivo efficacy was evaluated based on thickness and tensile strength of hair grown on previously shaved rat skin. Results show that the formulated 30% propolis-based cream had greater hair enhancing properties than the 10% propolis cream, which had a comparable effect with minoxidil.

Keywords: atomic absorption spectroscopy, differential scanning calorimetry (DSC), modified draize rabbit test, propolis

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Authors: Monu Verma, Hyunook Kim

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Heavy metals and organic dyes are the major sources of water pollution. Herein, a trifunctional β−cyclodextrin−ethylenediaminetetraacetic acid−chitosan (β−CD−EDTA−CS) polymer was synthesized using an easy and simple chemical route by the reaction of activated β−CD with CS through EDTA as a cross-linker (amidation reaction) for the removal of inorganic and organic pollutants from aqueous solution under different parameters such as pH, time effect, initial concentration, reusability, etc. The synthesized adsorbent was characterized using powder X-ray diffraction, Fourier transform infrared spectroscopy, field scanning electron microscopy, energy dispersive spectroscopy, Brunauer-Emmett-Teller (BET), thermogravimetric analyzer techniques to investigate their structural, functional, morphological, elemental compositions, surface area, and thermal properties, respectively. Two types of heavy metals, i.e., mercury (Hg²⁺) and cadmium (Cd²⁺), and three organic dyes, i.e., methylene blue (MB), crystal violet (CV), and safranin O (SO), were chosen as inorganic and organic pollutants, respectively, to study the adsorption capacity of β-CD-EDTA-CS in aqueous solution. The β-CD-EDTA-CS shows a monolayer adsorption capacity of 346.30 ± 14.0 and 202.90 ± 13.90 mg g−¹ for Hg²⁺ and Cd²⁺, respectively, and a heterogeneous adsorption capacity of 107.20 ± 5.70, 77.40 ± 5.30 and 55.30 ± 3.60 mg g−¹ for MB, CV and SO, respectively. Kinetics results followed pseudo-second order (PSO) kinetics behavior for both metal ions and dyes, and higher rate constants values (0.00161–0.00368 g mg−¹ min−¹) for dyes confirmed the cavitation of organic dyes (physisorption). In addition, we have also demonstrated the performance of β-CD-EDTA-CS for the four heavy metals, Hg²⁺, Cd²⁺, Ni²⁺, and Cu²⁺, and three dyes MB, CV, and SO in secondary treated wastewater. The findings of this study indicate that β-CD-EDTA-CS is simple and easy to synthesize and can be used in wastewater treatment.

Keywords: adsorption isotherms, adsorption mechanism, amino-β-cyclodextrin, heavy metal ions, organic dyes

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Authors: E. Gil, A. Zepeda, J. Rivera, C. Ben-Youssef, S. Rincón

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Water pollution has become one of the most serious environmental problems. Multiple methods have been proposed for the removal of Pb(II) from contaminated water. Among these, adsorption processes have shown to be more efficient, cheaper and easier to handle with respect to other treatment methods. However, research for adsorbents with high adsorption capacities is still necessary. For this purpose, we proposed in this work the study of metal-organic Framework [Co2(btec)(bipy)(DMF)2]n (MOF-Co) as adsorbent material of Pb (II) in aqueous media. MOF-Co was synthesized by a simple method. Firstly 4, 4’ dipyridyl, 1,2,4,5 benzenetetracarboxylic acid, cobalt (II) and nitrate hexahydrate were first mixed each one in N,N dimethylformamide (DMF) and then, mixed in a reactor altogether. The obtained solution was heated at 363 K in a muffle during 68 h to complete the synthesis. It was washed and dried, obtaining MOF-Co as the final product. MOF-Co was characterized before and after the adsorption process by Fourier transforms infrared spectra (FTIR) and X-ray photoelectron spectroscopy (XPS). The Pb(II) in aqueous media was detected by Absorption Atomic Spectroscopy (AA). In order to evaluate the adsorption process in the presence of Pb(II) in aqueous media, the experiments were realized in flask of 100 ml the work volume at 200 rpm, with different MOF-Co quantities (0.0125 and 0.025 g), pH (2-6), contact time (0.5-6 h) and temperature (298,308 and 318 K). The kinetic adsorption was represented by pseudo-second order model, which suggests that the adsorption took place through chemisorption or chemical adsorption. The best adsorption results were obtained at pH 5. Langmuir, Freundlich and BET equilibrium isotherms models were used to study the adsorption of Pb(II) with 0.0125 g of MOF-Co, in the presence of different concentration of Pb(II) (20-200 mg/L, 100 mL, pH 5) with 4 h of reaction. The correlation coefficients (R2) of the different models show that the Langmuir model is better than Freundlich and BET model with R2=0.97 and a maximum adsorption capacity of 833 mg/g. Therefore, the Langmuir model can be used to best describe the Pb(II) adsorption in monolayer behavior on the MOF-Co. This value is the highest when compared to other materials such as the graphene/activated carbon composite (217 mg/g), biomass fly ashes (96.8 mg/g), PVA/PAA gel (194.99 mg/g) and MOF with Ag12 nanoparticles (120 mg/g).

Keywords: adsorption, heavy metals, metal-organic frameworks, Pb(II)

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