Search results for: (FTIR) spectroscopy

Authors: Sylwia Orzechowska, Andrzej Wróbel, Eugeniusz Rokita

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The mineralization is a curious problem of connective tissues. Factors which may play a decisive role in the regulation of the yellow ligaments (YL) mineralization are still open questions. The aim of the studies was a detailed description of the chemical composition and morphology of mineral deposits in the human yellow ligaments. Investigations of the structural features of deposits were used to explain the impact of various factors on mineralization process. The studies were carried out on 24 YL samples, surgically removed from patients suffer from spinal canal stenosis and the patients who sustained a trauma. The micro-computed tomography was used to describe the morphology of mineral deposits. The X-ray fluorescence method and Fourier transform infrared spectroscopy were applied to determine the chemical composition of the samples. In order to eliminate the effect of blur in microtomographic images, the correction method of partial volume effect was used. The mineral deposits appear in 60% of YL samples, both in patients with a stenosis and following injury. The mineral deposits have a heterogeneous structure and they are a mixture of the tissue and mineral grains. The volume of mineral grains amounts to (1.9 ± 3.4)*10-3 mm3 while the density distribution of grains occurs in two distinct ranges (1.75 - 2.15 and 2.15-2.5) g/cm3. Application of the partial volume effect correction allows accurate calculations by eliminating the averaging effect of gray levels in tomographic images. The B-type carbonate-containing hydroxyapatite constitutes the mineral phase of majority YLs. The main phase of two samples was calcium pyrophosphate dihydrate (CPPD). The elemental composition of minerals in all samples is almost identical. This pathology may be independent on the spine diseases and it does not evoke canal stenosis. The two ranges of grains density indicate two stages of grains growth and the degree of maturity. The presence of CPPD crystals may coexist with other pathologies.

Keywords: FTIR, micro-tomography, mineralization, spinal ligaments

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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: Katarzyna Wal, Wojciech Stawiński, Piotr Rutkowski

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The scientific community is paying more and more attention to the problem of air pollution. Carbon dioxide is classified as one of the most harmful gases. Its emissions are generated during fossil fuel burning, waste management, and combustion and are responsible for global warming. Clay minerals constitute a group of promising materials for the role of adsorbents. They are composed of two types of phyllosilicate sheets: tetrahedral and octahedral, which form 1:1 or 2:1 structures. Vermiculite is one of their best-known representative, which can be used as an adsorbent from water and gaseous phase. The aim of the presented work was carbon dioxide adsorption on vermiculite. Acid-activated samples (W_NO3_x) were prepared by acid treatment with different concentrations of nitric acid (1, 2, 3, 4 mol L⁻¹). Vermiculite was subjected to modification in order to increase its porosity and adsorption properties. The prepared adsorbents were characterized using the BET-specific surface area analysis, thermogravimetry (TG), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Applied modifications significantly increase the specific surface area from 78,21 m² g⁻¹ for the unmodified sample (W_REF) to 536 m² g-1 for W_NO3_4. Obtained results showed that acid treatment tunes the material’s functional properties by increasing the contact surface and generating more active sites in its structure. The adsorption performance in terms carbon dioxide adsorption capacities follows the order of W_REF (25.91 mg g⁻¹) < W_NO3_1 (38.54 mg g⁻¹) < W_NO3_2 (44.03 mg g⁻¹) W_NO3_4 (67.51 mg g⁻¹) < W_NO3_3 (70.48 mg g⁻¹). Acid activation significantly improved the carbon dioxide adsorption properties of modified samples compared to raw material. These results demonstrate that vermiculite-based samples have the potential to be used as effective CO₂ adsorbents. Furthermore, acid treatment is a promising technique for improving the adsorption properties of clay minerals.

Keywords: adsorption, adsorbent, clay minerals, air pollution, environment

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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: Mohamed Abd Elfattah Ibraheem Elghrbawy

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Biodeterioration of cultural heritage is a complex process which is caused by the interaction of many physical, chemical and biological agents; the growth of microorganisms can cause staining, cracking, powdering, disfigurement and displacement of monuments material, which leads to the permanent loss of monuments material. Organisms causing biodeterioration on monuments have usually been controlled by chemical products (biocides). In order to overcome the impact of biocides on the environment, human health and monument substrates, alternative tools such as antimicrobial agents from natural products can be used for monuments conservation and protection. The problem is how to formulate antibacterial agents with high efficiency and low toxicity. Various types of biodegradable metal nanoparticles (MNPs) have many applications in plant extract delivery. So, Nano-encapsulation of metal and natural antimicrobial agents using polymers such as chitosan increases their efficacy, specificity and targeting ability. Green synthesis and characterization of metal nanoparticles such as silver with natural products extracted from some plants having antimicrobial properties, using the ecofriendly method one pot synthesis. Encapsulation of the new synthesized mixture using some biopolymers such as chitosan nanoparticles. The dispersions and homogeneity of the antimicrobial heterogeneous metal nanoparticles encapsulated by biopolymers will be characterized and confirmed by Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM) and Zeta seizer. The effect of the antimicrobial biopolymer metal nano-formulations on normal human cell lines will be investigated to evaluate the environmental safety of these formulations. The antimicrobial toxic activity of the biopolymeric antimicrobial metal nanoparticles formulations will be will be investigated to evaluate their efficiency towards different pathogenic bacteria and fungi.

Keywords: antimicrobial, biodeterioration, chitosan, cultural heritage, silver

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Authors: Syed Hadi Hasan, Devendra Kumar Singh, Viyaj Kumar

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Cr (VI) is a known toxic heavy metal and has been considered as a priority pollutant in water. The effluent of various industries including electroplating, anodizing baths, leather tanning, steel industries and chromium based catalyst are the major source of Cr (VI) contamination in the aquatic environment. Cr (VI) show high mobility in the environment and can easily penetrate cell membrane of the living tissues to exert noxious effects. The Cr (VI) contamination in drinking water causes various hazardous health effects to the human health such as cancer, skin and stomach irritation or ulceration, dermatitis, damage to liver, kidney circulation and nerve tissue damage. Herein, an attempt has been done to develop an efficient adsorbent for the removal of Cr (VI) from water. For this purpose nanosorbent composed of polyvinyl alcohol functionalized graphene oxide (GO/PVA) was prepared. Thus, obtained GO/PVA was characterized through FTIR, XRD, SEM, and Raman Spectroscopy. As prepared nanosorbent of GO/PVA was utilized for the removal Cr (VI) in batch mode experiment. The process variables such as contact time, initial Cr (VI) concentration, pH, and temperature were optimized. The maximum 99.8 % removal of Cr (VI) was achieved at initial Cr (VI) concentration 60 mg/L, pH 2, temperature 35 °C and equilibrium was achieved within 50 min. The two widely used isotherm models viz. Langmuir and Freundlich were analyzed using linear correlation coefficient (R2) and it was found that Langmuir model gives best fit with high value of R2 for the data of present adsorption system which indicate the monolayer adsorption of Cr (VI) on the GO/PVA. Kinetic studies were also conducted using pseudo-first order and pseudo-second order models and it was observed that chemosorptive pseudo-second order model described the kinetics of current adsorption system in better way with high value of correlation coefficient. Thermodynamic studies were also conducted and results showed that the adsorption was spontaneous and endothermic in nature.

Keywords: adsorption, GO/PVA, isotherm, kinetics, nanosorbent, thermodynamics

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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: Akhila Konala, Jagadeeswara Reddy Vennapusa, Sujay Chattopadhyay

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The energy consumption of humankind is growing day by day due to an increase in the population, industrialization and their needs for living. Fossil fuels are the major source of energy to satisfy energy needs, which are non-renewable energy resources. So, there is a need to develop green resources for energy production and storage. Phase change materials (PCMs) derived from plants (green resources) are well known for their capacity to store the thermal energy as latent heat during their phase change from solid to liquid. This property of PCM could be used for storage of thermal energy. In this study, a composite with fatty acid (caprylic acid; M.P 15°C, Enthalpy 179kJ/kg) as a phase change material and expanded perlite as support porous matrix was prepared through direct impregnation method for thermal energy storage applications. The prepared composite was characterized using Differential scanning calorimetry (DSC), Field Emission Scanning Electron Microscope (FESEM), Thermal Gravimetric Analysis (TGA), and Fourier Transform Infrared (FTIR) spectrometer. The melting point of the prepared composite was 15.65°C, and the melting enthalpy was 82kJ/kg. The surface nature of the perlite was observed through FESEM. It was observed that there are micro size pores in the perlite surface, which were responsible for the absorption of PCM into perlite. In TGA thermogram, the PCM loss from composite was started at ~90°C. FTIR curves proved there was no chemical interaction between the perlite and caprylic acid. So, the PCM composite prepared in this work could be effective to use in temperature maintenance of buildings.

Keywords: caprylic acid, composite, phase change materials, PCM, perlite, thermal energy

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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: 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: Daniela Rivera-Tobar Mario Perez-Won, Roberto Lemus-Mondaca, Gipsy Tabilo-Munizaga

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Different dietary trends worldwide seek to consume foods with anti-inflammatory properties, rich in antioxidants, proteins, and unsaturated fatty acids that lead to better metabolic, intestinal, mental, and cardiac health. In this sense, food matrices with high protein content based on macro and microalgae are an excellent alternative to meet the new needs of consumers. An emerging and environmentally friendly technology for producing protein matrices is ultrasonic agglomeration. It consists of the formation of permanent bonds between particles, improving the agglomeration of the matrix compared to conventionally agglomerated products (compression). Among the advantages of this process are the reduction of nutrient loss and the avoidance of binding agents. The objective of this research was to optimize the ultrasonic agglomeration process in matrices composed of Spirulina (Arthrospira platensis) powder and Cochayuyo (Durvillae Antartica) flour, by means of the response variable (Young's modulus) and the independent variables were the process conditions (percentage of ultrasonic amplitude: 70, 80 and 90; ultrasonic agglomeration times and cycles: 20, 25 and 30 seconds, and 3, 4 and 5). It was evaluated using a central composite design and analyzed using response surface methodology. In addition, the effects of agglomeration on thermophysical and microstructural properties were evaluated. It was determined that ultrasonic compression with 80 and 90% amplitude caused conformational changes according to Fourier infrared spectroscopy (FTIR) analysis, the best condition with respect to observed microstructure images (SEM) and differential scanning calorimetry (DSC) analysis, was the condition of 90% amplitude 25 and 30 seconds with 3 and 4 cycles of ultrasound. In conclusion, the agglomerated matrices present good macro and microstructural properties which would allow the design of food systems with better nutritional and functional properties.

Keywords: ultrasonic agglomeration, physical properties of food, protein matrices, macro and microalgae

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Authors: Saman Namvarrechi, Armin A. Dormeny, Javad Dargahi, Mojtaba Kahrizi

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Since last two decades, minimally invasive surgery (MIS) has grown significantly due to its advantages compared to the traditional open surgery like less physical pain, faster recovery time and better healing condition around incision regions; however, one of the important challenges in MIS is getting an effective sensing feedback within the patient’s body during operations. Therefore, surgeons need efficient tactile sensing like determining the hardness of contact tissue for investigating the patient’s health condition. In such a case, MIS tactile sensors are preferred to be able to provide force/pressure sensing, force position, lump detection, and softness sensing. Among different pressure sensor technologies, the piezoelectric operating principle is the fittest for MIS’s instruments, such as catheters. Using PVDF with its copolymer, TrFE, as a piezoelectric material, is a common method of design and fabrication of a tactile sensor due to its ease of implantation and biocompatibility. In this research, PVDF-TrFE polymer is deposited via spin-coating method and treated with various post-deposition processes to investigate its piezoelectricity and amount of electroactive β phase. These processes include different post thermal annealing, the effect of spin-coating speed, different layer of deposition, and the presence of additional hydrate salt. According to FTIR spectroscopy and SEM images, the amount of the β phase and porosity of each sample is determined. In addition, the optimum experimental study is established by considering every aspect of the fabrication process. This study clearly shows the effective way of deposition and fabrication of a tactile PVDF-TrFE based sensor and an enhancement methodology to have a higher β phase and piezoelectric constant in order to have a better sense of touch at the end effector of biomedical devices.

Keywords: β phase, minimally invasive surgery, piezoelectricity, PVDF-TrFE, tactile sensor

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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: Golam Saklayen, Sheikh Rashel al Ahmed, Ferdous Rahman, Ismail Abu Bakar

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Investigation on Lanthanum Fluoride LaF3 layer embedding Silicon Nanocrystals (Si-NCs) fabricated using a novel one-step chemical method has been reported in this presentation. Application of this material has been tested for low-voltage operating non-volatile memory and Schottkey-junction solar cell. Colloidal solution of Si-NCs in hydrofluoric acid (HF) was prepared from meso-porous silicon by ultrasonic vibration (sonication). This solution prevents the Si-NCs to be oxidized. On a silicon (Si) substrate, LaCl3 solution in HCl is allowed to react with the colloidal solution of prepared Si-NCs. Since this solution contains HF, LaCl3 reacts with HF and produces LaF3 crystals that deposits on the silicon substrate as a layer embedding Si-NCs. This a novel single step chemical way of depositing LaF3 insulating layer embedding Si-NCs. The X-Ray diffraction of the deposited layer shows a polycrystalline LaF3 deposition on silicon. A non-stoichiometric LaF3 layer embedding Si-NCs was found by EDX analysis. The presence of Si-NCs was confirmed by SEM. FTIR spectroscopy of the deposited LaF3 powder also confirmed the presence of Si-NCs. The size of Si-NCs was found to be inversely proportional to the ultrasonic power. After depositing proper contacts on the back of Si and LaF3, the devices have been tested as a non-volatile memory and solar cell. A memory window of 525 mV was obtained at a programming and erasing bias of 2V. The LaF3 films with Si NCs showed strong absorption and was also found to decrease optical transmittance than pure LaF3 film of same thickness. The I-V characteristics of the films showed a dependency on the incident light intensity where current changed under various light illumination. Experimental results show a lot of promise for Si-NCs-embedded LaF3 layer to be used as an insulating layer in MIS devices as well as an photoactive material in Schottkey junction solar cells.

Keywords: silicon nanocrystals (Si NCs), LaF3, colloidal solution, Schottky junction solar cell

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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: M. Nazem Salimi, C. Abrinia, M. Baniassadi, M. Ehsani

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Mechanical properties of epoxy based nanocomposites containing copper coated MWCNTs were investigated and a comparative study between nanocomposites containing functionalized MWCNTs and copper coated MWCNTs which are already functionalized was conducted. The MWCNTs was deposited with copper nanoparticles through electroless deposition process after accomplishment of "two-step" method as sensitization and activation procedures on oxidized MWCNTs. In addition, functionalization of MWCNTs was carried out through combination of two covalent and non-covalent funcionalization methods using HNO3 for acid solution of covalent treatment and Triton X100 as non-ionic surfactant of non-covalent treatment. The presence of functional groups and removal of impurities of MWCNTs were confirmed by FTIR and Raman spectroscopy, respectively. The layer of copper nanoparticles on the MWCNTs wall increasing its diameter was observed by SEM. Utilizing solution blending process, 0.1%, 0.5% and 1.5% wt loading of both copper coated MWCNTs and non-coated MWCNTs were used to prepare epoxy-based nanocomposites. The tensile, flexural and impact properties of nanocomposites were investigated. The results of tensile test demonstrated that nanocomposites containing copper coated MWCNTs exhibited brittle behavior compared to those reinforced with functionalized MWCNTs, whereas former one exhibited higher values of modulus than latter one for concentrations more than 0.4% wt. Presence of copper particles on MWCNTs surface decreased the tensile strength of nanocomposites. In comparison to pure epoxy, nanocomposites with treated-MWCNTs and Cu-MWCNTs loading of 0.1% wt showed an increase of 35% and 51.6% for flexural strength beside 20% and 30% increase in flexural modulus, respectively, whereas flexural properties of both naocomposites decreased with increasing of CNTs concentration. The results of impact strength of nanocomposites with Cu-CNTs demonstrated that impact properties decreased with increasing of filler content with a optimum value at 0.1% wt while in high concentrations impact properties of Cu-nanocomposites exhibited lower values than f-MWCNT nanocomposites.

Keywords: epoxyresin, nanocomposite, functionalization, copper, electroless deposition process, mechanical properties

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Authors: Omkar Gaonkar, Indumathi Nambi, Suresh G. Kumar

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The functional and morphological aspects of soil structure determine the soil quality. The dispersion of colloidal soil particles, especially the clay fraction and rupture of soil aggregates, both of which play an important role in soil structure development, lead to degradation of soil quality. The main objective of this work was to determine the effect of the behaviour of soil colloids on the agricultural soil structure and quality. The effect of commercial humic acid and soil natural organic matter on the electrical and structural properties of the soil colloids was also studied. Agricultural soil, belonging to the sandy loam texture class from northern part of India was considered in this study. In order to understand the changes in the soil quality in the presence and absence of humic acids, the soil fabric and structure was analyzed by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy (SEM). Electrical properties of natural soil colloids in aqueous suspensions were assessed by zeta potential measurements at varying pH values with and without the presence of humic acids. The influence of natural organic matter was analyzed by oxidizing the natural soil organic matter with hydrogen peroxide. The zeta potential of the soil colloids was found to be negative in the pH range studied. The results indicated that hydrogen peroxide treatment leads to deflocculation of colloidal soil particles. In addition, the humic acids undergoes effective adsorption onto the soil surface imparting more negative zeta potential to the colloidal soil particles. The soil hydrophilicity decreased in the presence of humic acids which was confirmed by surface free energy determination. Thus, it can be concluded that the presence of humic acids altered the soil fabric and structure, thereby affecting the soil quality. This study assumes significance in understanding soil aggregation and the interactions at soil solid-liquid interface.

Keywords: humic acids, natural organic matter, zeta potential, soil quality

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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: Julie Anne Braun, Leonardo D. da Fonseca, Gerson C. Parreira, Ricardo J. E. Andrade

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Polyurethanes (PU) are multifunctional polymers used across various industries. In construction, thermosetting polyurethanes are applied as coatings for flooring, paints, and waterproofing. They are widely specified in Brazil for waterproofing concrete structures like roof slabs and parking decks. Applied to concrete, they form a fully adhered membrane, providing a protective barrier with low water absorption, high chemical resistance, impermeability to liquids, and low vapor permeability. Their mechanical properties, including tensile strength (1 to 35 MPa) and Shore A hardness (83 to 88), depend on resin molecular weight and functionality, often using Methylene diphenyl diisocyanate. PU production, reliant on fossil-derived isocyanates and polyols, contributes significantly to carbon emissions. Sustainable alternatives, such as biopolyurethanes from renewable sources, are needed. Castor oil is a viable option for synthesizing sustainable polyurethanes. As a bio-based feedstock, castor oil is extensively cultivated in Brazil, making it a feasible option for the national market and ranking third internationally. This study aims to develop and characterize castor oil-based biopolyurethane for high-performance waterproofing and coating applications. A comparative analysis between castor oil-based PU and polyether polyol-based PU was conducted. Mechanical tests (tensile strength, Shore A hardness, abrasion resistance) and surface properties (contact angle, water absorption) were evaluated. Thermal, chemical, and morphological properties were assessed using thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The results demonstrated that both polyurethanes exhibited high mechanical strength. Specifically, the tensile strength for castor oil-based PU was 19.18 MPa, compared to 12.94 MPa for polyether polyol-based PU. Similarly, the elongation values were 146.90% for castor oil-based PU and 135.50% for polyether polyol-based PU. Both materials exhibited satisfactory performance in terms of abrasion resistance, with mass loss of 0.067% for castor oil PU and 0.043% for polyether polyol PU and Shore A hardness values of 89 and 86, respectively, indicating high surface hardness. The results of the water absorption and contact angle tests confirmed the hydrophilic nature of polyether polyol PU, with a contact angle of 58.73° and water absorption of 2.53%. Conversely, the castor oil-based PU exhibited hydrophobic properties, with a contact angle of 81.05° and water absorption of 0.45%. The results of the FTIR analysis indicated the absence of a peak around 2275 cm-1, which suggests that all of the NCO groups were consumed in the stoichiometric reaction. This conclusion is supported by the high mechanical test results. The TGA results indicated that polyether polyol PU demonstrated superior thermal stability, exhibiting a mass loss of 13% at the initial transition (around 310°C), in comparison to castor oil-based PU, which experienced a higher initial mass loss of 25% at 335°C. In summary, castor oil-based PU demonstrated mechanical properties comparable to polyether polyol PU, making it suitable for applications such as trafficable coatings. However, its higher hydrophobicity makes it more promising for watertightness. Increasing environmental concerns necessitate reducing reliance on non-renewable resources and mitigating the environmental impacts of polyurethane production. Castor oil is a viable option for sustainable polyurethanes, aligning with emission reduction goals and responsible use of natural resources.

Keywords: polyurethane, castor oil, sustainable, waterproofing, construction industry

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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: Monika Verma, Renuka Sharma, B. R. Gulati, Namita Singh

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In combination therapy, two chemotherapeutic agents work together in a collaborative action. It has appeared as one of the promising approaches to improve anti-cancer treatment efficacy. In the present investigation, piperine (P-NPS), paclitaxel (PTX NPS), and a combination of both, piperine-paclitaxel nanoparticle (Pip-PTX NPS), were made by the nanoprecipitation method and later characterized by PSA, DSC, SEM, TEM, and FTIR. All nanoparticles exhibited a monodispersed size distribution with a size of below 200 nm, zeta potential ranges from (-30-40mV) and a narrow polydispersity index (>0.3) of the drugs. The average encapsulation efficiency was found to be between 80 and 90%. In vitro release of drugs for nanoparticles was done spectrophotometrically. FTIR and DSC results confirmed the presence of the drug. The Pip-PTX NPS significantly inhibit cell proliferation as compared to the native drugs nanoparticles in the breast cancer cell line MCF-7. In addition, Pip-PTX NPS suppresses cells in colony formation and soft gel agar assay. Scratch migration and Transwell chamber invasion assays revealed that combined nanoparticles reduce the migration and invasion of breast cancer cells. Morphological studies showed that Pip-PTX NPS penetrates the cells and induces apoptosis, which was further confirmed by DNA fragmentation, SEM, and western blot analysis. Taken together, Pip-PTX NPS inhibits cell proliferation, anchorage dependent and anchorage independent cell growth, reduces migration and invasion, and induces apoptosis in cells. These findings support that combination therapy using Pip-PTX NPS represents a potential approach and could be helpful in the future for breast cancer therapy.

Keywords: piperine, paclitaxel, breast cancer, apoptosis

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Authors: El-Said I. El-Shafey, Syeda Naheed F. Ali, Saleh S. Al-Busafi, Haider A. J. Al-Lawati

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Date palm leaflets were utilized as a precursor for activated carbon (AC) preparation using KOH activation. AC produced was oxidized using nitric acid producing oxidized activated carbon (OAC). OAC that possesses acidic surface was surface functionalized to produce basic activated carbons using linear diamine compounds (ethylene diamine and propylene diamine). OAC was also functionalized to produce hydrophobic activated carbons using ethylamine (EA) and aniline (AN). Dehydrated carbon was also prepared from date palm leaflets using sulfuric acid dehydration/ oxidation and was surface functionalized in the same way as AC. Nitric acid oxidation was not necessary for DC as it is acidic carbon. The surface area of AC is high (823 m2/g) with microporosity domination, however, after oxidation and surface functionalization, both the surface area and surface microporosity decrease tremendously. DC surface area was low (15 m2/g) with mesoporosity domination. Surface functionalization has decreased the surface area of activated carbons. FTIR spectra show that -COOH group on DC and OAC almost disappeared after surface functionalization. The surface chemistry of all carbons produced was tested for pHzpc, basic sites, boehm titration, thermogravimetric analysis and zeta potential measurement. Scanning electron microscopy and energy dispersive spectroscopy in addition to CHN elemental analysis were also carried out. DC and OAC possess low pHzpc and high surface functionality, however, basic and hydrophobic carbons possess high pHzpc and low surface functionality. The different behavior of carbons is related to their different surface chemistry. Methylene blue adsorption was found to be faster on hydrophobic carbons based on AC and DC. The Larger adsorption capacity of methylene blue was found for hydrophobic carbons. Dominating adsorption forces of methylene blue varies from carbon to another depending on its surface nature. Sorption forces include hydrophobic forces, H-bonding, electrostatic interactions and van der Waals forces.

Keywords: carbon, acidic, basic, hydrophobic

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Authors: Ali Ayatic, Emad Mozaffari, Bahareh Tanhaei, Maryam Khajenoori, Saeedeh Movaghar Khoshkho, Ali Ayati

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The abuse of antibiotics, such as tetracycline (TC), is a great global threat to people and the use of topical antibiotics is a promising tact that can help to solve this problem. Antibiotic therapy is often appropriate and necessary for acute wound infections, while topical tetracycline can be highly efficient in improving the wound healing process in diabetics. Due to the advantages of drug-loaded hydrogels as wound dressing, such as ease of handling, high moisture resistance, excellent biocompatibility, and the ability to activate immune cells to speed wound healing, it was found as an ideal wound treatment. In this work, the tetracycline-loaded hydrogels combining agar (AG) and κ-carrageenan (k-CAR) as polymer materials were prepared, in which span60 surfactant was introduced inside as a drug carrier. The Field Emission Scanning Electron Microscopes (FESEM) and Fourier-transform infrared spectroscopy (FTIR) techniques were employed to provide detailed information on the morphology, composition, and structure of fabricated drug-loaded hydrogels and their mechanical properties, and hydrogel permeability to water vapor was investigated as well. Two types of gram-negative and gram-positive bacteria were used to explore the antibacterial properties of prepared tetracycline-contained hydrogels. Their swelling and drug release behavior was studied using the changing factors such as the ratio of polysaccharides (MAG/MCAR), the span60 surfactant concentration, potassium chloride (KCl) concentration and different release media (deionized water (DW), phosphate-buffered saline (PBS), and simulated wound fluid (SWF)) at different times. Finally, the kinetic behavior of hydrogel swelling was studied. Also, the experimental data of TC release to DW, PBS, and SWF using various mathematical models such as Higuchi, Korsmeyer-Peppas, zero-order, and first-order in the linear and nonlinear modes were evaluated.

Keywords: drug release, hydrogel, tetracycline, wound healing

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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: Shady S. Hassan, Brijesh K. Tiwari, Gwilym A. Williams, Amit K. Jaiswal

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Waste materials from a wide range of agro-industrial processes may be used as substrates for microbial growth, and subsequently the production of a range of high value products and bioenergy. In addition, utilization of these agro-residues in bioprocesses has the dual advantage of providing alternative substrates, as well as solving their disposal problems. Spent coffee grounds (SCG) are a by-product (45%) of coffee processing. SCG is a lignocellulosic material, which is composed mainly of cellulose, hemicelluloses, and lignin. Thus, a pretreatment process is required to facilitate an efficient enzymatic hydrolysis of such carbohydrates. In this context, microwave pretreatment of lignocellulosic biomass without the addition of harsh chemicals represents a green technology. Moreover, microwave treatment has a high heating efficiency and is easy to implement. Thus, microwave pretreatment of SCG without adding of harsh chemicals investigated as a green technology to enhance enzyme hydrolysis. In the present work, microwave pretreatment experiments were conducted on SCG at varying power levels (100, 250, 440, 600, and 1000 W) for 60 s. By increasing microwave power to a certain level (which vary by varying biomass), reducing sugar increases, then reducing sugar from biomass start to decrease with microwave power increase beyond this level. Microwave pretreatment of SCG at 60s followed by enzymatic hydrolysis resulted in total reducing sugars of 91.6 ± 7.0 mg/g of biomass (at microwave power of 100 w). Fourier transform Infrared Spectroscopy (FTIR) was employed to investigate changes in functional groups of biomass after pretreatment, while high-performance liquid chromatography (HPLC) was employed for determination of glucose. Pretreatment of lignocellulose using microwave was found to be an effective and energy efficient technology to improve saccharification and glucose yield. Energy performance will be evaluated for the microwave pretreatment, and the enzyme hydrolysate will be used as media component substitute for the production of ethanol and other high value products.

Keywords: lignocellulose, microwave, pretreatment, spent coffee grounds

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Authors: Kanika Kalra, Harmeet Kaur, Dinesh Goyal

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Total phenolics were extracted from waste orange peels by solvent extraction and alkali hydrolysis method. The most efficient solvents for extracting phenolic compounds from waste biomass were methanol (60%) > dimethyl sulfoxide > ethanol (60%) > distilled water. The extraction yields were significantly impacted by solvents (ethanol, methanol, and dimethyl sulfoxide) due to varying polarity and concentrations. Extraction of phenolics using 60% methanol yielded the highest phenolics (in terms of gallic acid equivalent (GAE) per gram of biomass) in orange peels. Alkali hydrolyzed extract from orange peels contained 7.58±0.33 mg GAE g⁻¹. By using the solvent extraction technique, it was observed that 60% methanol is comparatively the best-suited solvent for extracting polyphenolic compounds and gave the maximum yield of 4.68 ± 0.47 mg GAE g⁻¹ in orange peel extracts. DPPH radical scavenging activity and reducing the power of orange peel extract were checked, where 60% methanolic extract showed the highest antioxidant activity, 85.50±0.009% for DPPH, and dimethyl sulfoxide (DMSO) extract gave the highest yield of 1.75±0.01% for reducing power ability of the orange peels extract. Characterization of the polyphenolic compounds was done by using Fourier transformation infrared (FTIR) spectroscopy. Solvent and alkali hydrolysed extracts were evaluated for antibacterial activity using the agar well diffusion method against Gram-positive Bacillus subtilis MTCC441 and Gram-negative Escherichia coli MTCC729. Methanolic extract at 300µl concentration showed an inhibition zone of around 16.33±0.47 mm against Bacillus subtilis, whereas, for Escherichia coli, it was comparatively less. Broth-based turbidimetric assay revealed the antibacterial effect of different volumes of orange peel extracts against both organisms.

Keywords: orange peels, total phenolic content, antioxidant, antibacterial

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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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