Search results for: photothermal deflection spectroscopy

Authors: Fauzi Jarushi, Paul Cosentino, Edward Kalajian, Hadeel Dekhn

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At certain depths during large diameter displacement pile driving, rebound well over 0.25 inches was experienced, followed by a small permanent set during each hammer blow. High pile rebound (HPR) soils may stop the pile driving and results in a limited pile capacity. In some cases, rebound leads to pile damage, delaying the construction project, and the requiring foundations redesign. HPR was evaluated at seven Florida sites, during driving of square precast, prestressed concrete piles driven into saturated, fine silty to clayey sands and sandy clays. Pile Driving Analyzer (PDA) deflection versus time data recorded during installation, was used to develop correlations between cone penetrometer (CPT) pore-water pressures, pile displacements and rebound. At five sites where piles experienced excessive HPR with minimal set, the pore pressure yielded very high positive values of greater than 20 tsf. However, at the site where the pile rebounded, followed by an acceptable permanent set, the measured pore pressure ranged between 5 and 20 tsf. The pore pressure exhibited values of less than 5 tsf at the site where no rebound was noticed. In summary, direct correlations between CPTu pore pressure and rebound were produced, allowing identification of soils that produce HPR.

Keywords: CPTU, pore water pressure, pile rebound

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Authors: Adeleke G. E., Bello M. A., Abdulateef R. B., Olasinde T. T., Oriaje K. O., AransiI A., Elaigwu K. O., Omidoyin O. S., Shoyinka E. D., Awoyomi M. B., Akano M., Adaramoye O. A.

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Hymenocardia acidatul belongs to the genus, Hymenocardiaceae, which is widely distributed in Africa. Both the leaf and stem bark of the plant have been used in the treatment of several diseases. The present study examined the chemical constituents of the H. acida stem bark extract (HASBE) and its effects on some antioxidant indices and esterase enzymes in female Wistar rats. The HASBE was obtained by Soxhlet extraction using methanol and then subjected to Atomic Absorption Spectroscopy (AAS) for elemental analysis, and Fourier-Transform Infrared (FT-IR) spectroscopy, ultraviolet (UV) spectroscopy, for functional group analysis, while High-performance liquid chromatography (HPLC), and Gas Chromatography-Flame ionization detection (GC-FID) were carried out for compound identification. Forty-eight female Wistar rats were assigned into eight groups of six rats each and separately administered orally with normal saline (Control), 50, 100, 150, 200, 250, 300, 350 mg/kg of HASBE twice per week for eight weeks. The rats were sacrificed under chloroform anesthesia, and kidneys and heart were excised and processed to obtain homogenates. The levels of superoxide dismutase (SOD), catalase, Malondialdehyde (MDA), glutathione peroxidase (GPx), acetylcholinesterase (AChE), and carboxylesterase (CE) were determined spectrophotometrically. The AAS of HASBE shows the presence of eight elements, including Cobalt (0.303), Copper (0.222), Zinc (0.137), Iron (2.027), Nickel (1.304), Chromium (0.313), Manganese (0.213), and Magnesium (0.337 ppm). The FT-IR result of HASBE shows four peaks at 2961.4, 2926.0, 1056.7, and 1034.3 cm-1, while UV analysis shows a maximum absorbance (0.522) at 205 nm. The HPLC spectrum of HASBE indicates the presence of four major compounds, including orientin (77%), β-sitosterol (6.58%), rutin (5.02%), and betulinic acid (3.33%), while GC-FID result shows five major compounds, including rutin (53.27%), orientin (13.06%) and stigmasterol (11.73%), hymenocardine (6.43%) and homopterocarpin (5.29%). The SOD activity was significantly (p < 0.05) lowered in the kidney but elevated in the heart, while catalase was elevated in both organs relative to control rats. The GPx activity was significantly elevated only in the kidney, while MDA was not significantly (p > 0.05) affected in the two organs compared with controls. The activity of AChE was significantly elevated in both organs, while CE activity was elevated only in the kidney relative to control rats. The present study reveals that Hymenocardia acida stem bark extract majorly contains orientin, rutin, stigmasterol, hymenocardine, β-sitosterol, homopterocarpin, and betulinic acid. In addition, these compounds could possibly enhance redox status and esterase activities in the kidney and heart of Wistar rats.

Keywords: hymenocardia acida, elemental analysis, compounds identification, redox status, organs

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Authors: Sahin Yakut, H. Kemal Ulutas, Deniz Deger

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Plasma Assisted Physical Vapor Deposition (PAPVD) method used to produce Poly(ethylene oxide) (pPEO) thin films. Depositions were progressed at various plasma discharge powers as 0, 2, 5 and 30 W for pPEO at 500nm film thicknesses. The capacitance and dielectric dissipation of the thin films were measured at 0,1-107 Hz frequency range and 173-353 K temperature range by an impedance analyzer. Then, alternative conductivity (σac) and activation energies were derived from capacitance and dielectric dissipation. σac of conventional PEO (PEO precursor) was measured to determine the effect of plasma discharge. Differences were observed between the alternative conductivity of PEO’s and pPEO’s depending on plasma discharge power. By this purpose, structural characterization techniques such as Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied on pPEO thin films. Structural analysis showed that density of crosslinking is plasma power dependent. The crosslinking density increases with increasing plasma discharge power and this increase is displayed as increasing dynamic glass transition temperatures at DSC results. Also, shifting of frequencies of some type of bond vibrations, belonging to bond vibrations produced after fragmentation because of plasma discharge, were observed at FTIR results. The dynamic glass transition temperatures obtained from alternative conductivity results for pPEO consistent with the results of DSC. Activation energies exhibit Arrhenius behavior. Activation energies decrease with increasing plasma discharge power. This behavior supports the suggestion expressing that long polymer chains and long oligomers are fragmented into smaller oligomers or radicals.

Keywords: activation energy, dielectric spectroscopy, organic thin films, plasma polymer

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Authors: Totsaporn Suwannaruang, Kitirote Wantala

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The purposes of this research were to synthesize titanium dioxide photocatalyst doped with nitrogen (N-doped TiO₂) by hydrothermal method and to test the photocatalytic degradation of paraquat under UV and visible light illumination. The effect of calcination treatment temperature on their physical and chemical properties and photocatalytic efficiencies were also investigated. The characterizations of calcined N-doped TiO₂ photocatalysts such as specific surface area, textural properties, bandgap energy, surface morphology, crystallinity, phase structure, elements and state of charges were investigated by Brunauer, Emmett, Teller (BET) and Barrett, Joyner, Halenda (BJH) equations, UV-Visible diffuse reflectance spectroscopy (UV-Vis-DRS) by using the Kubelka-Munk theory, Wide-angle X-ray scattering (WAXS), Focussed ion beam scanning electron microscopy (FIB-SEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS), respectively. The results showed that the effect of calcination temperature was significant on surface morphology, crystallinity, specific surface area, pore size diameter, bandgap energy and nitrogen content level, but insignificant on phase structure and oxidation state of titanium (Ti) atom. The N-doped TiO₂ samples illustrated only anatase crystalline phase due to nitrogen dopant in TiO₂ restrained the phase transformation from anatase to rutile. The samples presented the nanorice-like morphology. The expansion on the particle was found at 650 and 700°C of calcination temperature, resulting in increased pore size diameter. The bandgap energy was determined by Kubelka-Munk theory to be in the range 3.07-3.18 eV, which appeared slightly lower than anatase standard (3.20 eV), resulting in the nitrogen dopant could modify the optical absorption edge of TiO₂ from UV to visible light region. The nitrogen content was observed at 100, 300 and 400°C only. Also, the nitrogen element disappeared at 500°C onwards. The nitrogen (N) atom can be incorporated in TiO₂ structure with the interstitial site. The uncalcined (100°C) sample displayed the highest percent paraquat degradation under UV and visible light irradiation due to this sample revealed both the highest specific surface area and nitrogen content level. Moreover, percent paraquat removal significantly decreased with increasing calcination treatment temperature. The nitrogen content level in TiO₂ accelerated the rate of reaction with combining the effect of the specific surface area that generated the electrons and holes during illuminated with light. Therefore, the specific surface area and nitrogen content level demonstrated the important roles in the photocatalytic activity of paraquat under UV and visible light illumination.

Keywords: restraining phase transformation, interstitial site, chemical charge state, photocatalysis, paraquat degradation

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Authors: Abdulsamee Halahla, Emad Allout

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The purpose of this research is to study the behavior of exterior beam-column joints (BCJs) strengthened with ultra-high performance concrete (UHPC), in terms of the shear strength and maximum displacement using pushover analysis at the tip of the beam. A finite element (F.E) analysis was performed to study three main parameters – the level of the axial load in the column (N), the beam shear reinforcement (Av/s)B, and the effect of using UHPC. The normal concrete at the studied joint region was replaced by UHPC. The model was verified by using experimental results taken from the literature. The results showed that the UHPC contributed to the transference of the plastic hinge from the joint to the beam-column interface. In addition, the strength of the UHPC-strengthened joints was enhanced dramatically from 8% to 38% for the joints subjected to 12.8MPa and zero axial loads, respectively. Moreover, the UHPC contributed in improving the maximum deflection. This improvement amounted to 1% and 176% for the joints subjected to zero and 12.8MPa axial load, respectively.

Keywords: ultra high performance concrete, ductility, reinforced concrete joints, finite element modeling, nonlinear behavior; pushover analysis

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Authors: L. Cesari, L. Canabady-Rochelle, F. Mutelet

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The thermal conversion of lignin produces bio-oils that contain many compounds with high added-value such as phenolic compounds. In order to efficiently extract these compounds, the possible use of choline bis(trifluoromethylsulfonyl)imide [Choline][NTf2] ionic liquid was explored. To this end, a multistep approach was implemented. First, binary (phenolic compound and solvent) and ternary (phenolic compound and solvent and ionic liquid) solutions were investigated. Eight binary systems of phenolic compound and water were investigated at atmospheric pressure. These systems were quantified using the turbidity method and UV-spectroscopy. Ternary systems (phenolic compound and water and [Choline][NTf2]) were investigated at room temperature and atmospheric pressure. After stirring, the solutions were let to settle down, and a sample of each phase was collected. The analysis of the phases was performed using gas chromatography with an internal standard. These results were used to quantify the values of the interaction parameters of thermodynamic models. Then, extractions were performed on synthetic solutions to determine the influence of several operating conditions (temperature, kinetics, amount of [Choline][NTf2]). With this knowledge, it has been possible to design and simulate an extraction process composed of one extraction column and one flash. Finally, the extraction efficiency of [Choline][NTf2] was quantified with real bio-oils from lignin pyrolysis. Qualitative and quantitative analysis were performed using gas chromatographic connected to mass spectroscopy and flame ionization detector. The experimental measurements show that the extraction of phenolic compounds is efficient at room temperature, quick and does not require a high amount of [Choline][NTf2]. Moreover, the simulations of the extraction process demonstrate that [Choline][NTf2] process requires less energy than an organic one. Finally, the efficiency of [Choline][NTf2] was confirmed in real situations with the experiments on lignin pyrolysis bio-oils.

Keywords: bio-oils, extraction, lignin, phenolic compounds

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: Sharon Waichman, Shahaf Froim, Ido Zukerman, Shmuel Barzilai, Shmual Hayun, Avi Raveh

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Boron carbide is a ceramic material with superior properties such as high chemical and thermal stability, high hardness and high wear resistance. Moreover, it has a big cross section for neutron absorption and therefore can be employed in nuclear based applications. However, an efficient attachment of boron carbide to a metal such as aluminum can be very challenging, mainly because of the formation of aluminum-carbon bonds that are unstable in humid environment, the affinity of oxygen to the metal and the different thermal expansion coefficients of the two materials that may cause internal stresses and a subsequent failure of the bond. Here, we aimed to achieving a strong and a durable attachment between the boron carbide coating and the aluminum substrate. For this purpose, we applied Ti as a thin intermediate layer that provides a gradual change in the thermal expansion coefficients of the configured layers. This layer is continuous and therefore prevents the formation of aluminum-carbon bonds. Boron carbide coatings with a thickness of 1-5 µm were deposited on the aluminum substrate by pulse-DC magnetron sputtering. Prior to the deposition of the boron carbide layer, the surface was pretreated by energetic ion plasma followed by deposition of the Ti intermediate adhesive layer in a continuous process. The properties of the Ti intermediate layer were adjusted by the bias applied to the substrate. The boron carbide/aluminum bond was evaluated by various methods and complementary techniques, such as SEM/EDS, XRD, XPS, FTIR spectroscopy and Glow Discharge Spectroscopy (GDS), in order to explore the structure, composition and the properties of the layers and to study the adherence mechanism of the boron carbide/aluminum contact. Based on the interfacial bond characteristics, we propose a desirable solution for improved adhesion of boron carbide to aluminum using a highly efficient intermediate adhesive layer.

Keywords: adhesion, boron carbide coatings, ceramic/metal bond, intermediate layer, pulsed-DC magnetron sputtering

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Authors: Neha Thakur, Pravin S. More

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The interaction of CO, H2 and LPG with Cu-dosed SnO2 catalysts was studied by means of Fourier transform infrared spectroscopy (FTIR). With increasing Cu loading, pronounced and progressive red shifts of the C–O stretching frequency associated with molecular CO adsorbed on the Cu/SnO2 component were observed. This decrease in n(CO) correlates with enhancement of CO dissociation at higher temperatures on Cu promoted SnO2 catalysts under conditions, where clean Cu is almost ineffective. In the conclusion, the capability of our technique is discussed, and a technique for enhancing the sensitivity in our technique is proposed.

Keywords: FTIR, spectroscopic, dissociation, n(CO)

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Authors: Seyed Amin Vakili, Sahar Sadat Vakili, Seyed Ehsan Vakili, Nader Abdoli Yazdi

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The main purpose of this paper is to present the Modified Newmark Method as a method of non-linear frame analysis by considering the effect of the axial load (second order analysis). The discussion will be restricted to plane frameworks containing a constant cross-section for each element. In addition, it is assumed that the frames are prevented from out-of-plane deflection. This part of the investigation is performed to generalize the established method for the assemblage structures such as frameworks. As explained, the governing differential equations are non-linear and cannot be formulated easily due to unknown axial load of the struts in the frame. By the assumption of constant axial load, the governing equations are changed to linear ones in most methods. Since the modeling and the solutions of the non-linear form of the governing equations are cumbersome, the linear form of the equations would be used in the established method. However, according to the ability of the method to reconsider the minor omitted parameters in modeling during the solution procedure, the axial load in the elements at each stage of the iteration can be computed and applied in the next stage. Therefore, the ability of the method to present an accurate approach to the solutions of non-linear equations will be demonstrated again in this paper.

Keywords: nonlinear, stability, buckling, modified newmark method

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Authors: Wafa Jahouach-Rabai, Khouloud Ouerghi, Zohra Azzouz-Berriche, Faouzi Hosni

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Widely used organic products in the pharmaceutical industry have been detected in environmental systems, essentially carboxylic acids. In this purpose, the degradation efficiency of these contaminants was evaluated using an advanced oxidation process (AOP), namely ionization process as an alternative to conventional water treatment technologies. This process permitted the generation of radical reactions to directly degrade organic pollutants in wastewater. In fact, gamma irradiation of aqueous solutions produces several reactive radicals, essentially hydroxyl radical (OH), to destroy recalcitrant pollutants. Different concentrations of aqueous solutions of Fumaric acid (FA) were considered in this study (0.1-1 mmol/L), which were treated by irradiation doses from 1 to 15 kGy with 6.1 kGy/h rate by ionizing system in pilot scale (⁶⁰Co irradiator). Variations of main parameters influencing degradation efficiency versus absorbed doses were released in the aim to optimize total mineralization of considered pollutants. Preliminary degradation pathway until complete mineralization into CO₂ has been suggested based on detection of residual degradation derivatives using different techniques, namely high performance liquid chromatography (HPLC) and electron paramagnetic resonance spectroscopy (EPR). Results revealed total destruction of treated compound, which improve the efficiency of this process in water remediation. We investigated the reactivity of hydroxyl radicals generated by irradiation on dicarboxylic acid (FA) in aqueous solutions, leading to its degradation into other smaller molecules. In fact, gamma irradiation of FA leads to the formation of hydroxylated intermediates such as hydroxycarbonyl radical which were identified by EPR spectroscopy. Finally, pilot plant irradiation facilities improved the applicability of radiation technology on large scale.

Keywords: AOP, radiolysis, fumaric acid, gamma irradiation, hydroxyl radical, EPR, HPLC

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Authors: Radka Gorejova, Ivana Sisolakova, Jana Shepa, Frederika Chovancova, Renata Orinakova

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Diabetes mellitus (DM) is a serious metabolic disease characterized by chronic hyperglycemia. Often, the symptoms are not sufficiently observable at early stages, and so hyperglycemia causes pathological and functional changes before the diagnosis of the DM. Therefore, the development of an electrochemical sensor that will be fast, accurate, and instrumentally undemanding is currently needful. Screen-printed carbon electrodes (SPCEs) can be considered as the most suitable matrix material for insulin sensors because of the small size of the working electrode. It leads to the analyst's volume reduction to only 50 µl for each measurement. The surface of bare SPCE was modified by a combination of chitosan, multi-walled carbon nanotubes (MWCNTs), and zinc nanoparticles (ZnNPs) to obtain better electrocatalytic activity towards insulin oxidation. ZnNPs were electrochemically deposited on the chitosan-MWCNTs/SPCE surface using the pulse deposition method. Thereafter, insulin was determined on the prepared electrode using chronoamperometry and electrochemical impedance spectroscopy (EIS). The chronoamperometric measurement was performed by adding a constant amount of insulin in 0.1 M NaOH and PBS (2 μl) with the concentration of 2 μM, and the current response of the system was monitored after a gradual increase in concentration. Subsequently, the limit of detection (LOD) of the prepared electrode was determined via the Randles-Ševčík equation. The LOD was 0.47 µM. Prepared electrodes were studied also as the impedimetric sensors for insulin determination. Therefore, various insulin concentrations were determined via EIS. Based on the performed measurements, the ZnNPs/chitosan-MWCNTs/SPCE can be considered as a potential candidate for novel electrochemical sensor for insulin determination. Acknowledgments: This work has been supported by the projects Visegradfund project number 22020140, VEGA 1/0095/21 of the Slovak Scientific Grant Agency, and APVV-PP-COVID-20-0036 of the Slovak Research and Development Agency.

Keywords: zinc nanoparticles, insulin, chronoamperometry, electrochemical impedance spectroscopy

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Authors: Khaled Sandjak, Boualem Tiliouine

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Structural analysis of flexible pavements has been and still is currently performed using multi-layer elastic theory. However, for thinly surfaced pavements subjected to low to medium volumes of traffics, the importance of non-linear stress-strain behaviour of unbound granular materials (UGM) requires the use of more sophisticated numerical models for structural design and performance of such pavements. In the present work, nonlinear unbound aggregates constitutive model is implemented within an axisymmetric finite element code developed to simulate the nonlinear behaviour of pavement structures including two local aggregates of different mineralogical nature, typically used in Algerian pavements. The performance of the mechanical model is examined about its capability of representing adequately, under various conditions, the granular material non-linearity in pavement analysis. In addition, deflection data collected by falling weight deflectometer (FWD) are incorporated into the analysis in order to assess the sensitivity of critical pavement design criteria and pavement design life to the constitutive model. Finally, conclusions of engineering significance are formulated.

Keywords: FWD backcalculations, finite element simulations, Nonlinear resilient behaviour, pavement response and performance, RLT test results, unbound granular materials

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Authors: Hamza Ouachtouk, Amine Harbi, Said Azerblou, Youssef Naimi, El Mostafa Tace

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This study delves into the structural, vibrational, magnetic, and electronic properties of La₂MMnO₆ double perovskites, where M denotes Ni, Co, and Zn. Recognized for their versatile ionic configurations within the A and B sub-lattices, double perovskite oxides have attracted considerable interest due to their extensive array of physical properties, which include multiferroic behavior, colossal magnetoresistance, and ferroelectric/piezoelectric functionalities. These materials are pivotal for energy-related technologies like solid oxide fuel cells and water-splitting catalysis, attributed to their superior oxygen ion transport and storage capabilities. This research places particular emphasis on La₂NiMnO₆ and La₂CoMnO₆, known for their distinct magnetic, electric, and multiferroic properties, and extends the investigation to La₂ZnMnO₆, synthesized via high-temperature solid-state chemistry. This addition aims to ascertain the impact of zinc substitution on these properties. Structural analysis through X-ray diffraction has confirmed a monoclinic structure within the P2₁/n space group. Comprehensive vibrational studies utilizing infrared and Raman spectroscopy, alongside additional XRD assessments, provide a detailed examination of the dynamic and electronic behaviors of these compounds. The results underscore the significant role of chemical composition in modulating their functional properties. Comparatively, this study highlights that zinc substitution notably alters the electronic and magnetic responses, which could enhance the applicability of these materials in advanced energy technologies. This expanded analysis not only reinforces our understanding of La₂MMnO₆'s physical characteristics but also highlights its potential applications in the next generation of energy solutions.

Keywords: double perovskites, structural analysis, vibrational spectroscopy, magnetic properties, electronic properties, high-temperature solid-state chemistry, La₂MMnO₆, monoclinic structure, x-ray diffraction

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Authors: A. Zuchowska, A. Buta, M. Mazurkiewicz-Pawlicka, A. Malolepszy, L. Stobinski, Z. Brzozka

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In recent years, graphene-based materials are finding more and more applications in biological science. As a thin, tough, transparent and chemically resistant materials, they appear to be a very good material for the production of implants and biosensors. Interest in graphene derivatives also resulted at the beginning of research about the possibility of their application in cancer therapy. Currently, the analysis of their potential use in photothermal therapy and as a drug carrier is mostly performed. Moreover, the direct anticancer properties of graphene-based materials are also tested. Nowadays, cytotoxic studies are conducted on in vitro cell culture in standard culture vessels (macroscale). However, in this type of cell culture, the cells grow on the synthetic surface in static conditions. For this reason, cell culture in macroscale does not reflect in vivo environment. The microfluidic systems, called Lab-on-a-chip, are proposed as a solution for improvement of cytotoxicity analysis of new compounds. Here, we present the evaluation of cytotoxic properties of graphene oxide (GO) on breast, liver and colon cancer cell line in a microfluidic system in two spatial models (2D and 3D). Before cell introduction, the microchambers surface was modified by the fibronectin (2D, monolayer) and poly(vinyl alcohol) (3D, spheroids) covering. After spheroid creation (3D) and cell attachment (2D, monolayer) the selected concentration of GO was introduced into microsystems. Then monolayer and spheroids viability/proliferation using alamarBlue® assay and standard microplate reader was checked for three days. Moreover, in every day of the culture, the morphological changes of cells were determined using microscopic analysis. Additionally, on the last day of the culture differential staining using Calcein AM and Propidium iodide were performed. We were able to note that the GO has an influence on all tested cell line viability in both monolayer and spheroid arrangement. We showed that GO caused higher viability/proliferation decrease for spheroids than a monolayer (this was observed for all tested cell lines). Higher cytotoxicity of GO on spheroid culture can be caused by different geometry of the microchambers for 2D and 3D cell cultures. Probably, GO was removed from the flat microchambers for 2D culture. Those results were also confirmed by differential staining. Comparing our results with the studies conducted in the macroscale, we also proved that the cytotoxic properties of GO are changed depending on the cell culture conditions (static/ flow).

Keywords: cytotoxicity, graphene oxide, monolayer, spheroid

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Authors: N. A. Hamizi, M. R. Johan, Y. H. Hor, A. N. Sabri, Y. Y. A. Yong

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In this research, Mn-doped CdSe QDs is synthesized by using paraffin liquid as the reacting solvent and oleic acid as the ligands for Cd in order to produce Mn-doped CdSe QDs in zinc-blende crystal structure. Characterization studies for synthesized Mn-doped CdSe QDs are carried out using UV-visible and photoluminescence spectroscopy. The absorption wavelengths in UV-vis test and emission wavelengths in PL test were increase with the increases in the ripening temperature and time respectively.

Keywords: semiconductor, chemical synthesis, optical properties, ripening

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Authors: Laura C. Loaiza, Elodie Salager, Nicolas Louvain, Athmane Boulaoued, Antonella Iadecola, Patrik Johansson, Lorenzo Stievano, Vincent Seznec, Laure Monconduit

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Lithium-ion batteries (LIBs) have an important place among energy storage devices due to their high capacity and good cyclability. However, the advancements in portable and transportation applications have extended the research towards new horizons, and today the development is hampered, e.g., by the capacity of the electrodes employed. Silicon and germanium are among the considered modern anode materials as they can undergo alloying reactions with lithium while delivering high capacities. It has been demonstrated that silicon in its highest lithiated state can deliver up to ten times more capacity than graphite (372 mAh/g): 4200 mAh/g for Li₂₂Si₅ and 3579 mAh/g for Li₁₅Si₄, respectively. On the other hand, germanium presents a capacity of 1384 mAh/g for Li₁₅Ge₄, and a better electronic conductivity and Li ion diffusivity as compared to Si. Nonetheless, the commercialization potential of Ge is limited by its cost. The synergetic effect of Si₁₋ₓGeₓ alloys has been proven, the capacity is increased compared to Ge-rich electrodes and the capacity retention is increased compared to Si-rich electrodes, but the exact performance of this type of electrodes will depend on factors like specific capacity, C-rates, cost, etc. There are several reports on various formulations of Si₁₋ₓGeₓ alloys with promising LIB anode performance with most work performed on complex nanostructures resulting from synthesis efforts implying high cost. In the present work, we studied the electrochemical mechanism of the Si₀.₅Ge₀.₅ alloy as a realistic micron-sized electrode formulation using carboxymethyl cellulose (CMC) as the binder. A combination of a large set of in situ and operando techniques were employed to investigate the structural evolution of Si₀.₅Ge₀.₅ during lithiation and delithiation processes: powder X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), Raman spectroscopy, and 7Li solid state nuclear magnetic resonance spectroscopy (NMR). The results have presented a whole view of the structural modifications induced by the lithiation/delithiation processes. The Si₀.₅Ge₀.₅ amorphization was observed at the beginning of discharge. Further lithiation induces the formation of a-Liₓ(Si/Ge) intermediates and the crystallization of Li₁₅(Si₀.₅Ge₀.₅)₄ at the end of the discharge. At really low voltages a reversible process of overlithiation and formation of Li₁₅₊δ(Si₀.₅Ge₀.₅)₄ was identified and related with a structural evolution of Li₁₅(Si₀.₅Ge₀.₅)₄. Upon charge, the c-Li₁₅(Si₀.₅Ge₀.₅)₄ was transformed into a-Liₓ(Si/Ge) intermediates. At the end of the process an amorphous phase assigned to a-SiₓGey was recovered. Thereby, it was demonstrated that Si and Ge are collectively active along the cycling process, upon discharge with the formation of a ternary Li₁₅(Si₀.₅Ge₀.₅)₄ phase (with a step of overlithiation) and upon charge with the rebuilding of the a-Si-Ge phase. This process is undoubtedly behind the enhanced performance of Si₀.₅Ge₀.₅ compared to a physical mixture of Si and Ge.

Keywords: lithium ion battery, silicon germanium anode, in situ characterization, X-Ray diffraction

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Authors: Pudji Astuti, C. P. C. Putro, C. M. Airin, L. Sjahfirdi, S. Widiyanto, H. Maheshwari

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Stress of slaughter animals starting long before until at the time of process of slaughtering which cause misery and decrease of meat quality. Meanwhile, determination of animal stress using hormonal such as cortisol is expensive and less practical so that portable stress indicator for cows based on Fourier Transform Infrared Spectroscopy (FTIR) must be provided. The aims of this research are to find out the comparison process of slaughter between Rope Casting Local (RCL) and Restraining Box Method (RBM) by measuring of cortisol and wavelength in FTIR methods. Thirty two of male Ongole crossbred cattle were used in this experiment. Blood sampling was taken from jugular vein when they were rested and repeated when slaughtered. All of blood samples were centrifuged at 3000 rpm for 20 minutes to get serum, and then divided into two parts for cortisol assayed using ELISA and for measuring the wavelength using FTIR. The serum then measured at the wavelength between 4000-400 cm-1 using MB3000 FTIR. Band data absorption in wavelength of FTIR is analyzed descriptively by using FTIR Horizon MBTM. For RCL, average of serum cortisol when the animals rested were 11.47 ± 4.88 ng/mL, when the time of slaughter were 23.27 ± 7.84 ng/mL. For RBM, level of cortisol when rested animals were 13.67 ± 3.41 ng/mL and 53.47 ± 20.25 ng/mL during the slaughter. Based on student t-Test, there were significantly different between RBM and RCL methods when beef cattle were slaughtered (P < 0.05), but no significantly different when animals were rested (P > 0.05). Result of FTIR with the various of wavelength such as methyl group (=CH3) 2986cm-1, methylene (=CH2) 2827 cm-1, hydroxyl (-OH) 3371 cm-1, carbonyl (ketones) (C=O) 1636 cm-1, carboxyl (COO-1) 1408 cm-1, glucosa 1057 cm-1, urea 1011 cm-1have been obtained. It can be concluded that the RCL slaughtered method is better than the RBM method based on the increase of cortisol as an indicator of stress in beef cattle (P<0.05). FTIR is really possible to be used as stub of stress tool due to differentiate of resting and slaughter condition by recognizing the increase of absorption and the separation of component group at the wavelength.

Keywords: cows, cortisol, FTIR, RBM, RCL, stress indicator

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Authors: M. Al-Farttoosi, M. Y. Rafiq, J. Summerscales, C. Williams

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Structures can be subjected to impact loading from various sources like earthquake, tsunami, missiles and explosions. The impact loading can cause different degrees of damage to concrete structures. The demand for strengthening and rehabilitation of damaged structures is increasing. In recent years, Car0bon Fibre Reinforced Polymer (CFRP) matrix composites has gain more attention for strengthening and repairing these structures. To study the impact behaviour of the reinforced concrete (RC) beams strengthened or repaired using CFRP, a heavy impact test machine was designed and manufactured .The machine included a newly designed support system for beams together with various instrumentation. This paper describes the support design configuration of the impact test machine, instrumentation and dynamic analysis of the concrete beams. To evaluate the efficiency of the new impact test machine, experimental impact tests were conducted on simple supported reinforced concrete beam. Different methods were used to determine the impact force and impact response of the RC beams in terms of inertia force, maximum deflection, reaction force and fracture energy. The manufactured impact test machine was successfully used in testing RC beams under impact loading and used successfully to test the reinforced concrete beams strengthened or repaired using CFRP under impact loading.

Keywords: beam, concrete, impact, machine

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Authors: Naamane Remita, Mohammed laïd Mechri, Nouredine Zekri, Smaïl Chihi

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The goal of this study is the estimation real and imaginary components of both electrical impedance and permittivity z', z'' and ε', ε'' respectively, in Ouargla dunes sand at different temperatures and different frequencies, with alternating current (AC) equal to 1 volt, using the impedance spectroscopy (IS). This method is simple and non-destructive. the results can frequently be correlated with a number of physical properties, dielectric properties and the impacts of the composition on the electrical conductivity of solids. The experimental results revealed that the real part of impedance is higher at higher temperature in the lower frequency region and gradually decreases with increasing frequency. As for the high frequencies, all the values of the real part of the impedance were positive. But at low frequency the values of the imaginary part were positive at all temperatures except for 1200 degrees which were negative. As for the medium frequencies, the reactance values were negative at temperatures 25, 400, 200 and 600 degrees, and then became positive at the rest of the temperatures. At high frequencies of the order of MHz, the values of the imaginary part of the electrical impedance were in contrast to what we recorded for the middle frequencies. The results showed that the electrical permittivity decreases with increasing frequency, at low frequency we recorded permittivity values of 10+ 11, and at medium frequencies it was 10+ 07, while at high frequencies it was 10+ 02. The values of the real part of the electrical permittivity were taken large values at the temperatures of 200 and 600 degrees Celsius and at the lowest frequency, while the smallest value for the permittivity was recorded at the temperature of 400 degrees Celsius at the highest frequency. The results showed that there are large values of the imaginary part of the electrical permittivity at the lowest frequency and then it starts decreasing as the latter increases (the higher the frequency the lower the values of the imaginary part of the electrical permittivity). The character of electrical impedance variation indicated an opportunity to realize the polarization of Ouargla dunes sand and acquaintance if this compound consumes or produces energy. It’s also possible to know the satisfactory of equivalent electric circuit, whether it’s miles induction or capacitance.

Keywords: electrical impedance, electrical permittivity, temperature, impedance spectroscopy, dunes sand ouargla

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Authors: Mezidi Amar

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In this research work, crack propagation at the interface of a composite beam is considered. The behavior of composite beams (CB) depends upon a law based on relationship between tangential or normal efforts with inelastic propagation. Throughout this study, composite beams are classified like composite beams with partial connection or sandwich beams of three layers. These structural systems are controlled by the same nature of differential equations regarding their behavior in the plane, as well as out-of-plane. Multi-layer elements with partial connection are typically met in the field of timber construction where the elements are assembled by joining. The formalism of the behavior in the plane and out-of-plane of these composite beams is obtained and their results concerning the engineering aspect or simple of interpretation are proposed for the case of composite beams made up of rectangular section and simply supported section. An apparent analytical peculiarity or paradox in the bending behavior of elastic–composite beams with interlayer slip, sandwich beam or other similar problems subjected to boundary moments exists. For a fully composite beam subjected to end moments, the partial composite model will render a non-vanishing uniform value for the normal force in the individual subelement. Obtained results are similar to those for the case of vibrations in the plane as well for the composite beams as for the sandwich beams where eigen-frequencies increase with related rigidity.

Keywords: composite beam, behaviour, interface, deflection, propagation

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Authors: Pratima Kumari, Sukha Ranjan Samadder

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This research aims to contribute to the sustainable production of graphene materials by exploring the extraction of graphite from spent primary and secondary batteries. The increasing demand for graphene materials, a versatile and high-performance material, necessitates environmentally friendly methods for its synthesis. The process involves a well-planned methodology, beginning with the gathering and categorization of batteries, followed by the disassembly and careful removal of graphite from anode structures. The use of environmentally friendly solvents and mechanical techniques ensures an efficient and eco-friendly extraction of graphite. Advanced approaches such as the modified Hummers' method and chemical reduction process are utilized for the synthesis of graphene materials, with a focus on optimizing parameters. Various analytical techniques such as Fourier-transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, and Raman spectroscopy were employed to validate the quality and structure of the produced graphene materials. The major findings of this study reveal the successful implementation of the methodology, leading to the production of high-quality graphene materials suitable for advanced material applications. Thorough characterization using various advanced techniques validates the structural integrity and purity of the graphene. The economic viability of the process is demonstrated through a comprehensive economic analysis, highlighting the potential for large-scale production. This research contributes to the field of sustainable production of graphene materials by offering a systematic methodology that efficiently transforms spent batteries into valuable graphene resources. Furthermore, the findings not only showcase the potential for upcycling electronic waste but also address the pressing need for environmentally conscious processes in advanced material synthesis.

Keywords: spent primary batteries, spent secondary batteries, graphite extraction, advanced material synthesis, circular economy approach

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Authors: András Szekrényes

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Delamination is one of the major failure modes in laminated composite structures. Delamination tips are mostly captured by spatial numerical models in order to predict crack growth. This paper presents some mechanical models of delaminated composite shells based on shallow shell theories. The mechanical fields are based on a third-order displacement field in terms of the through-thickness coordinate of the laminated shell. The undelaminated and delaminated parts are captured by separate models and the continuity and boundary conditions are also formulated in a general way providing a large size boundary value problem. The system of differential equations is solved by the state space method for an elliptic delaminated shell having simply supported edges. The comparison of the proposed and a numerical model indicates that the primary indicator of the model is the deflection, the secondary is the widthwise distribution of the energy release rate. The model is promising and suitable to determine accurately the J-integral distribution along the delamination front. Based on the proposed model it is also possible to develop finite elements which are able to replace the computationally expensive spatial models of delaminated structures.

Keywords: J-integral, levy method, third-order shell theory, state space solution

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Authors: Mustapha A. Tijjani, Fanna I. Abdulrahman, Irfan Z. Khan, Umar K. Sandabe, Cong Li

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Air dried sample V. doniana after collection and identification was extracted with ethanol and further partition with chloroform, ethyl acetate and n-butanol. Ethanolic extract (11.9g) was fractionated on a silica gel accelerated column chromatography using solvents such as n-hexane, ethyl acetate and methanol. Each eluent fractions (150ml aliquots) were collected and monitored with thin layer chromatography. Fractions with similar Rf values from same solvents system were pooled together. Phytochemical test of all the fractions were performed using standard procedure. Complete elution yielded 48 fractions (150ml/fraction) which were pooled to 24 fractions base on the Rf values. It was further recombined and 12 fractions were obtained on the basis on Rf values and coded Vd1 to Vd12 fractions. Vd8 was further eluted with ethylacetate and methanol and gave fourteen sub fractions Vd8-a, -Vd8-m. Fraction Vd8-a (56mg) gave a white crystal compound coded V1. It was further checked on TLC and observed under ultraviolet lamp and was found to give a single spot. The Rf values were calculated to be 0.433. The melting point was determined using Gallenkamp capillary melting point apparatus and found to be 241-243°C uncorrected. Characterization of the isolated compound coded V1 was done using FT-infra-red spectroscopy, HNMR, 13CNMR(1and 2D) and HRESI-MS. The IR spectrum of compound V1 shows prominent peaks that corresponds to OHstr (3365cm-1) and C=0 (1652cm-1) etc. This spectrum suggests that among the functional moiety in compound V1 are the carbonyl and hydroxyl group. The 1H NMR (400 MHz) spectrum of compound V1 in DMSO-d6 displayed five singlet signals at δ 0.72 (3H, s, H-18), 0.79 (3H, s, H-19), 1.03 (3H, s, H-21), 1.04 (3H, s, H-26), 1.06 (3H, s, H-27) each integrating for three protons indicating the five methyl functional groups present in the compound. It further showed a broad singlet at δ 5.58 integrated for 1 H due to an olefinic H-atom adjacent to the carbonyl carbon atom. Three signals at δ 3.10 (d, J = 9.0 Hz, H-22), 3.59 (m, 1H, 2H-a) and 3.72 (m, 1H, 3H-e), each integrating for one proton is due to oxymethine protons indicating that three oxymethine H-atoms are present in the compound. These all signals are characteristic to the ecdysteroid skeletons. The 13C-NMR spectrum showed the presence of 27 carbon atoms, suggesting that may be steroid skeleton. The DEPT-135 experiment showed the presence of five CH3, eight CH2, and seven CH groups, and seven quaternary C-atoms. The molecular formula was established as C27H44O7 by high resolution electron spray ionization-mass spectroscopy (HRESI-MS) positive ion mode m/z 481.3179. The signals in mass spectrum are 463, 445, and 427 peaks corresponding to losses of one, two, three, or four water molecules characteristic for ecdysterone skeleton reported in the literature. Based on the spectral analysis (HNMR, 13CNMR, DEPT, HMQC, IR, HRESI-MS) the compound V1 is thus concluded to have ecdysteriod skeleton and conclusively conforms with 2β, 3β 14α, 20R, 22R, 25-hexahydroxy-5 β cholest-7-ene-6- one, or 2, 3, 14, 20, 22, 25 hexahydroxy cholest-7-ene-6-one commonly known as 20-hydroxyecdysone.

Keywords: vitex, phytochemical, purification, isolation, chromatography, spectroscopy

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Authors: Lorenzo Cocola, Massimo Fedel, Dragiša Savić, Bojana Danilović, Luca Poletto

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An instrument for the detection and evaluation of gaseous carbon dioxide in the headspace of closed containers has been developed in the context of Packsensor Italian-Serbian joint project. The device is based on Tunable Diode Laser Absorption Spectroscopy (TDLAS) with a Wavelength Modulation Spectroscopy (WMS) technique in order to accomplish a non-invasive measurement inside closed containers of fermented dairy products (yogurts and fermented cheese in cups and bottles). The purpose of this instrument is the continuous monitoring of carbon dioxide concentration during incubation and storage of products over a time span of the whole shelf life of the product, in the presence of different microorganisms. The instrument’s optical front end has been designed to be integrated in a thermally stabilized incubator. An embedded computer provides processing of spectral artifacts and storage of an arbitrary set of calibration data allowing a properly calibrated measurement on many samples (cups and bottles) of different shapes and sizes commonly found in the retail distribution. A calibration protocol has been developed in order to be able to calibrate the instrument on the field also on containers which are notoriously difficult to seal properly. This calibration protocol is described and evaluated against reference measurements obtained through an industry standard (sampling) carbon dioxide metering technique. Some sets of validation test measurements on different containers are reported. Two test recordings of carbon dioxide concentration evolution are shown as an example of instrument operation. The first demonstrates the ability to monitor a rapid yeast growth in a contaminated sample through the increase of headspace carbon dioxide. Another experiment shows the dissolution transient with a non-saturated liquid medium in presence of a carbon dioxide rich headspace atmosphere.

Keywords: TDLAS, carbon dioxide, cups, headspace, measurement

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Authors: Chung-Hao Wu, Tung-Dju Lin, Ming-Chin Ho, Minehiro Nishiyama

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This paper discusses reported fire tests of concrete beams and columns, future fire tests of beam/column frames, and an innovative concept for designing a beam/column furnace. The proposed furnace could be designed to maximize the efficiency of fire test procedures and minimize the cost of furnace construction and fuel consumption. ASTM E119 and ISO 834 standards were drafted based on prescriptive codes and have several weaknesses. The first involves a provision allowing the support regions of a test element to be protected from fire exposure. The second deals with the L/30 deflection end point instead of the structural end point (collapse) in order to protect the hydraulic rams from fire damage. Furthermore, designers commonly use the measured fire endurances of interior columns to assess fire ratings of edge and corner columns of the same building. The validity of such an engineering practice is theoretically unsound. Performance-Based Codes (PBC) require verification tests of structural frames including the beam/column joints to overcome these weaknesses but allow the use of element test data as reference only. In the last 30 years, PBC have gained global popularity because the innovative design and flexibility in achieving an ultimate performance goal.

Keywords: fire resistance, concrete structure, beam/column frame, fire tests

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Authors: S. A. Tabatabaei, S. Aarabi

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Predicting the hot mix asphalt (HMA) response and performance is a challenging task because of the subjectivity of HMA under the complex loading and environmental condition. The behavior of HMA is a function of temperature of loading and also shows the time and rate-dependent behavior directly affecting design criteria of mixture. Velocity of load passing make the time and rate. The viscoelasticity illustrates the reaction of HMA under loading and environmental conditions such as temperature and moisture effect. The behavior has direct effect on design criteria such as tensional strain and vertical deflection. In this paper, the computational framework for viscoelasticity and implementation in 3D dimensional HMA model is introduced to use in finite element method. The model was lied under various repeated loading conditions at constant temperature. The response of HMA viscoelastic behavior is investigated in loading condition under speed vehicle and sensitivity of behavior to the range of speed and compared to HMA which is supposed to have elastic behavior as in conventional design methods. The results show the importance of loading time pulse, unloading time and various speeds on design criteria. Also the importance of memory fading of material to storing the strain and stress due to repeated loading was shown. The model was simulated by ABAQUS finite element package

Keywords: viscoelasticity, finite element method, repeated loading, HMA

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Authors: W. Thongkham, K. Sinthiptharakoon, K. Tantisantisom, A. Klamchuen, P. Khanchaitit, K. Jiramitmongkon, C. Lertsatitthanakorn, M. Liangruksa

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Due to demands of sustainable energy, thermoelectricity converting waste heat into electrical energy has become one of the intensive fields of worldwide research. However, such harvesting technology has shown low device performance in the temperature range below 150℃. In this work, a hybrid nanowire of inorganic bismuth telluride (Bi₂Te₃) and organic poly(3,4-ethylenedioxythiophene):polystyrenesulfonate (PEDOT:PSS) synthesized using a simple in-situ one-pot synthesis, enhancing efficiency of the nanowire-incorporated PEDOT:PSS-based thermoelectric converter is highlighted. Since the improvement is ascribed to the increased electrical conductivity of the thermoelectric host material, the individual hybrid nanowires are investigated using voltage-dependent conductive atomic force microscopy (CAFM) and spectroscopy (CAFS) considering that the electrical transport measurement can be performed either on insulating or conducting areas of the sample. Correlated with detailed chemical information on the crystalline structure and compositional profile of the nanowire core-shell structure, an electrical transporting pathway through the nanowire and the corresponding electronic-band structure have been determined, in which the native oxide layer on the Bi₂Te₃ surface is not considered, and charge conduction on the topological surface states of Bi₂Te₃ is suggested. Analyzing the core-shell nanowire synthesized using the conventional mixing of as-prepared Bi₂Te₃ nanowire with PEDOT:PSS for comparison, the oxide-removal effect of the in-situ encapsulating polymeric layer is further supported. The finding not only provides a structural information for mechanistic determination of the thermoelectricity, but it also encourages new approach toward more appropriate encapsulation and consequently higher efficiency of the nanowire-based thermoelectric generation.

Keywords: electrical transport measurement, hybrid Bi₂Te₃-PEDOT:PSS nanowire, nanoencapsulation, thermoelectricity, topological insulator

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Authors: Mercedes Bertotto, Marcelo Bello, Hector Goicoechea, Veronica Fusca

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The National Service of Agri-Food Health and Quality (SENASA), controls honey to detect contamination by synthetic or natural chemical substances and establishes and controls the traceability of the product. The utility of near-infrared spectroscopy for the detection of adulteration of honey with high fructose corn syrup (HFCS) was investigated. First of all, a mixture of different authentic artisanal Argentinian honey was prepared to cover as much heterogeneity as possible. Then, mixtures were prepared by adding different concentrations of high fructose corn syrup (HFCS) to samples of the honey pool. 237 samples were used, 108 of them were authentic honey and 129 samples corresponded to honey adulterated with HFCS between 1 and 10%. They were stored unrefrigerated from time of production until scanning and were not filtered after receipt in the laboratory. Immediately prior to spectral collection, honey was incubated at 40°C overnight to dissolve any crystalline material, manually stirred to achieve homogeneity and adjusted to a standard solids content (70° Brix) with distilled water. Adulterant solutions were also adjusted to 70° Brix. Samples were measured by NIR spectroscopy in the range of 650 to 7000 cm⁻¹. The technique of specular reflectance was used, with a lens aperture range of 150 mm. Pretreatment of the spectra was performed by Standard Normal Variate (SNV). The ant colony optimization genetic algorithm sample selection (ACOGASS) graphical interface was used, using MATLAB version 5.3, to select the variables with the greatest discriminating power. The data set was divided into a validation set and a calibration set, using the Kennard-Stone (KS) algorithm. A combined method of Potential Functions (PF) was chosen together with Partial Least Square Linear Discriminant Analysis (PLS-DA). Different estimators of the predictive capacity of the model were compared, which were obtained using a decreasing number of groups, which implies more demanding validation conditions. The optimal number of latent variables was selected as the number associated with the minimum error and the smallest number of unassigned samples. Once the optimal number of latent variables was defined, we proceeded to apply the model to the training samples. With the calibrated model for the training samples, we proceeded to study the validation samples. The calibrated model that combines the potential function methods and PLSDA can be considered reliable and stable since its performance in future samples is expected to be comparable to that achieved for the training samples. By use of Potential Functions (PF) and Partial Least Square Linear Discriminant Analysis (PLS-DA) classification, authentic honey and honey adulterated with HFCS could be identified with a correct classification rate of 97.9%. The results showed that NIR in combination with the PT and PLS-DS methods can be a simple, fast and low-cost technique for the detection of HFCS in honey with high sensitivity and power of discrimination.

Keywords: adulteration, multivariate analysis, potential functions, regression

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: electron diffraction spectroscopy, high strength concrete, interfacial transition zone, normal strength concrete, scanning electron microscopy

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