Search results for: in situ Raman Spectroscopy

Authors: J. J. Rickard, A. Belli, P. Goldberg Oppenheimer

Abstract:

Medical diagnostics, environmental monitoring, homeland security and forensics increasingly demand specific and field-deployable analytical technologies for quick point-of-care diagnostics. Although technological advancements have made optical methods well-suited for miniaturization, a highly-sensitive detection technique for minute sample volumes is required. Raman spectroscopy is a well-known analytical tool, but has very weak signals and hence is unsuitable for trace level analysis. Enhancement via localized optical fields (surface plasmons resonances) on nanoscale metallic materials generates huge signals in surface-enhanced Raman scattering (SERS), enabling single molecule detection. This enhancement can be tuned by manipulation of the surface roughness and architecture at the sub-micron level. Nevertheless, the development and application of SERS has been inhibited by the irreproducibility and complexity of fabrication routes. The ability to generate straightforward, cost-effective, multiplex-able and addressable SERS substrates with high enhancements is of profound interest for SERS-based sensing devices. While most SERS substrates are manufactured by conventional lithographic methods, the development of a cost-effective approach to create nanostructured surfaces is a much sought-after goal in the SERS community. Here, a method is established to create controlled, self-organized, hierarchical nanostructures using electrohydrodynamic (HEHD) instabilities. The created structures are readily fine-tuned, which is an important requirement for optimizing SERS to obtain the highest enhancements. HEHD pattern formation enables the fabrication of multiscale 3D structured arrays as SERS-active platforms. Importantly, each of the HEHD-patterned individual structural units yield a considerable SERS enhancement. This enables each single unit to function as an isolated sensor. Each of the formed structures can be effectively tuned and tailored to provide high SERS enhancement, while arising from different HEHD morphologies. The HEHD fabrication of sub-micrometer architectures is straightforward and robust, providing an elegant route for high-throughput biological and chemical sensing. The superior detection properties and the ability to fabricate SERS substrates on the miniaturized scale, will facilitate the development of advanced and novel opto-fluidic devices, such as portable detection systems, and will offer numerous applications in biomedical diagnostics, forensics, ecological warfare and homeland security.

Keywords: hierarchical electrohydrodynamic patterning, medical diagnostics, point-of care devices, SERS

Procedia PDF Downloads 317

Authors: Jadranka Blazhevska Gilev

Abstract:

IR laser-induced ablation of poly(butylacrylate-methylmethacrylate/hydroxyl ethyl methacrylate)/reduced graphene oxide (p(BA/MMA/HEMA)/rGO) was examined with 0.5, 0.75 and 1 wt% reduced graphene oxide content in relation to polymer. The irradiation was performed with TEA (transversely excited atmosphere) CO₂ laser using incident fluence of 15-20 J/cm², repetition frequency of 1 Hz, in an evacuated (10-3 Pa) Pyrex spherical vessel. Thin deposited nanocomposites films with large specific area were obtained using different substrates. The properties of the films deposited on these substrates were evaluated by TGA, FTIR, (Thermogravimetric analysis, Fourier Transformation Infrared) Raman spectroscopy and SEM microscopy. Homogeneous distribution of graphene sheets was observed from the SEM images, making polymer/rGO deposit an ideal candidate for SERS application. SERS measurements were performed using Rhodamine 6G as probe molecule on the substrate Ag/p(BA/MMA/HEMA)/rGO.

Keywords: laser ablation, reduced graphene oxide, polymer/rGO nanocomposites, thin deposited film

Procedia PDF Downloads 165

Authors: Hakan Gungunes, Ismail A. Auwal, Abdulhadi Baykal, Sagar E. Shirsath

Abstract:

Barium hexaferrite, BaFe₁₂O₁₉, substituted by Bi³⁺ and La³⁺ (BaBiₓLaₓFe₁₂₋₂ₓO₁₉ where 0.0 ≤ x ≤ 0.5) were prepared by solid state synthesis route. The effect of substituted Bi³⁺ and La³⁺ ions on the structure, morphology, magnetic and cation distributions of barium hexaferrite were investigated by X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR) and Mössbauer spectroscopy. XRD powder patterns were refined by the Rietveld analysis method which confirmed the formation of single phase magneto-plumbite structure and the substitution of La³⁺ and Bi³⁺ ions into the lattice of barium ferrite. These results show that both La³⁺ and Bi³⁺ ions completely enter into barium hexaferrite lattice without disturbing the hexagonal ferrite structure. The EDX spectra confirmed the presence of all the constituents in expected elemental percentage. From 57Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values on Bi and La substitutions have been determined. Cation distribution in the presently investigated hexaferrite system was estimated using the relative area of Mössbauer spectroscopy.

Keywords: hexaferrite, mössbauer, cation distribution, solid state synthesis

Procedia PDF Downloads 337

Authors: Ziwei Song, Junjun Fan, Jeremy Teo, Yang Yu, Yukun Ma, Jie Yan, Shupei Mo, Lisa Tucker-Kellogg, Peter So, Hanry Yu

Abstract:

Liver is the center of detoxification and exposed to toxic metabolites all the time. It is highly regenerative after injury, with the ability to restore even after 70% partial hepatectomy. Most of the previous studies were using hepatectomy as injury models for liver regeneration study. There is limited understanding of small-scale liver injury, which can be caused by either low dose drug consumption or hepatocyte routine metabolism. Although these small in situ injuries do not cause immediate symptoms, repeated injuries will lead to aberrant wound healing in liver. Therefore, the cellular dynamics during liver regeneration is critical for our understanding of liver regeneration mechanism. We aim to study the liver regeneration of small-scale in situ liver injury in transgenic mice labeling actin (Lifeact-GFP). Previous studies have been using sample sections and biopsies of liver, which lack real-time information. In order to trace every individual hepatocyte during the regeneration process, we have developed and optimized an intravital imaging system that allows in vivo imaging of mouse liver for consecutive 5 days, allowing real-time cellular tracking and quantification of hepatocytes. We used femtosecond-laser ablation to make controlled and repeatable liver injury model, which mimics the real-life small in situ liver injury. This injury model is the first case of its kind for in vivo study on liver. We found that small-scale in situ liver injury is repaired by the coordination of hypertrophy and migration of hepatocytes. Hypertrophy is only transient at initial phase, while migration is the main driving force to complete the regeneration process. From cellular aspect, Akt/mTOR pathway is activated immediately after injury, which leads to transient hepatocyte hypertrophy. From mechano-sensing aspect, the actin cable, formed at apical surface of wound proximal hepatocytes, provides mechanical tension for hepatocyte migration. This study provides important information on both chemical and mechanical signals that promote liver regeneration of small in situ injury. We conclude that hypertrophy and migration play a dominant role at different stages of liver regeneration.

Keywords: hepatocyte, hypertrophy, intravital imaging, liver regeneration, migration

Procedia PDF Downloads 182

Authors: M. Sikoń, E. Bidzińska

Abstract:

An attempt to apply EPR (Electron Paramagnetic Resonance) spectroscopy to experimental analysis of the mechanical state of the loaded material is considered in this work. Theory concerns the participation of electrons in transfer of mechanical action. The model of measurement is shown by applying classical mechanics and quantum mechanics. Theoretical analysis is verified using EPR spectroscopy twice, once for the free spacemen and once for the mechanical loaded spacemen. Positive results in the form of different spectra for free and loaded materials are used to describe the mechanical state in continuum based on statistical mechanics. Perturbation of the optical electrons in the field of the mechanical interactions inspires us to propose new optical properties of the materials with mechanical stresses.

Keywords: Cosserat medium, EPR spectroscopy, optical active electrons, optical activity

Procedia PDF Downloads 347

Authors: Surjyakanta Rana, Sreekantha B. Jonnalagadda

Abstract:

Synthesis of well distributed Pd nanoparticles (3 – 7 nm) on organo amine-functionalized graphene is reported, which demonstrated excellent catalytic activity towards Suzuki coupling reaction. The active material was characterized by X-ray diffraction (XRD), BET surface area, X-ray photoelectron spectra (XPS), Fourier-transfer infrared spectroscopy (FTIR), Raman spectra, Scanning electron microscope (SEM), Transmittance electron microscopy (TEM) analysis and HRTEM. FT-IR revealed that the organic amine functional group was successfully grafted onto the graphene oxide surface. The formation of palladium nanoparticles was confirmed by XPS, TEM and HRTEM techniques. The catalytic activity in the coupling reaction was superb with 100% conversion and 98 % yield and also activity remained almost unaltered up to six cycles. Typically, an extremely high turnover frequency of 185,078 h-1 is observed in the C-C Suzuki coupling reaction using organo di-amine functionalized graphene as catalyst.

Keywords: Di-amine, graphene, Pd nanoparticle, suzuki coupling

Procedia PDF Downloads 347

Authors: Reem M. Altuwirqi, Mohja S. Summan, Entesar A. Ganash, Safia H. Hamidalddin, Tamer E. Youssef, Mohammed A. Gondal

Abstract:

Laser-Induced Breakdown Spectroscopy (LIBS) technique using 1064 nm Nd: YAG laser was optimized and applied for investigating the existence of radioactive elements (uranium) in twenty-six different ceramic tiles. These tiles were collected from the local Saudi market. Qualitative and quantitative analysis for trace radioactive elements like uranium in these samples was achieved using LIBS. The plasma parameters such as temperature and electron density were calculated to confirm that the plasma generated by the tile samples under laser irradiation can be related to analyte concentrations. In order to perform a quantitative analysis, calibration curves were constructed for two uranium lines (U II (424.166 nm) and U II (424.437 nm)). The Uranium activity concentration in Bq/kg for each sample was measured. Cross-validation of LIBS results with a conventional technique such as Gamma-Ray spectroscopy was also carried out for five ceramic samples. The results show that the LIBS method is an effective way of determining radioactive elements such as uranium in ceramic tiles. Moreover, the uranium concentrations of the investigated samples were below the permissible safe limit for building materials in the majority of samples. Such LIBS system could be applied to determine the presence of natural radioactive elements in ceramic tiles and their radioactivity level rapidly to ensure that they are under the safe allowed limit.

Keywords: laser-induced breakdown spectroscopy, gamma-ray spectroscopy, natural radioactivity, uranium, ceramic tiles

Procedia PDF Downloads 140

Authors: Sergei Zhevnenko

Abstract:

Сontinuous layer of tantalum boride is formed on the surface as a result of reactive wetting of oxidized tantalum by copper melt with boron at a temperatures above 1150 °C. An increase in the wetting temperature above 1400 °C leads to a change in the formation mechanism of tantalum borides, they are formed in the nanosized flakes. In the presented work, we studied the process of copper-based in-situ composite formation, strengthened by the particles of tantalum borides. We investigated the structure of the formed particles, the conditions, and the kinetics of their formation. Dissolving boride particles do not have time to mix uniformly in the melt upon sufficiently rapid cooling and form a macrostructure, partly repeating the shape of the metallic tantalum. This allows to set different gradient structures in the copper alloy. Such macrostructures have been obtained. Boride particles and microstructures were studied by scanning and transmission electron microscopy, and regions with particles were investigated by nanoindentation. In this work, we also measured the kinetics of impregnation of porous tantalum with copper-boron melt and studied the structures of the composite, in which the melt filling the interpore space is saturated with boride particles.

Keywords: copper, tantalum borides, in-situ composites, wetting, imbibition

Procedia PDF Downloads 69

Authors: Assamen Ayalew Ejigu, Liang-Chiun Chao

Abstract:

In recent semiconductor and nanotechnology, quality material synthesis, proper characterizations, and productions are the big challenges. As cuprous oxide (Cu2O) is a promising semiconductor material for photovoltaic (PV) and other optoelectronic applications, this study was aimed at to grow and characterize high quality Cu2O nanorods for the improvement of the efficiencies of thin film solar cells and other potential applications. In this study, well-structured cuprous oxide (Cu2O) nanorods were successfully fabricated using IBSD method in which the Cu2O samples were grown on silicon substrates with a substrate temperature of 400°C in an IBSD chamber of pressure of 4.5 x 10-5 torr using copper as a target material. Argon, and oxygen gases were used as a sputter and reactive gases, respectively. The characterization of the Cu2O nanorods (NRs) were done in comparison with Cu2O thin film (TF) deposited with the same method but with different Ar:O2 flow rates. With Ar:O2 ratio of 9:1 single phase pure polycrystalline Cu2O NRs with diameter of ~500 nm and length of ~4.5 µm were grow. Increasing the oxygen flow rates, pure single phase polycrystalline Cu2O thin film (TF) was found at Ar:O2 ratio of 6:1. The field emission electron microscope (FE-SEM) measurements showed that both samples have smooth morphologies. X-ray diffraction and Rama scattering measurements reveals the presence of single phase Cu2O in both samples. The differences in Raman scattering and photoluminescence (PL) bands of the two samples were also investigated and the results showed us there are differences in intensities, in number of bands and in band positions. Raman characterization shows that the Cu2O NRs sample has pronounced Raman band intensities, higher numbers of Raman bands than the Cu2O TF which has only one second overtone Raman signal at 2 (217 cm-1). The temperature dependent photoluminescence (PL) spectra measurements, showed that the defect luminescent band centered at 720 nm (1.72 eV) is the dominant one for the Cu2O NRs and the 640 nm (1.937 eV) band was the only PL band observed from the Cu2O TF. The difference in optical and structural properties of the samples comes from the oxygen flow rate change in the process window of the samples deposition. This gave us a roadmap for further investigation of the electrical and other optical properties for the tunable fabrication of the Cu2O nano/micro structured sample for the improvement of the efficiencies of thin film solar cells in addition to other potential applications. Finally, the novel morphologies, excellent structural and optical properties seen exhibits the grown Cu2O NRs sample has enough quality to be used in further research of the nano/micro structured semiconductor materials.

Keywords: defect levels, nanorods, photoluminescence, Raman modes

Procedia PDF Downloads 195

Authors: Ömer Tamer, Davut Avcı, Yusuf Atalay

Abstract:

Novel picolinate complex of manganese(II) ion, [Mn(pic)2] [pic: picolinate or 2-pyridinecarboxylate], was prepared and fully characterized by single crystal X-ray structure determination. The manganese(II) complex was characterized by FT-IR, FT-Raman and UV–Vis spectroscopic techniques. The C=O, C=N and C=C stretching vibrations were found to be strong and simultaneously active in IR and spectra. In order to support these experimental techniques, density functional theory (DFT) calculations were performed at Gaussian 09W. Although the supramolecular interactions have some influences on the molecular geometry in solid state phase, the calculated data show that the predicted geometries can reproduce the structural parameters. The molecular modeling and calculations of IR, Raman and UV-vis spectra were performed by using DFT levels. Nonlinear optical (NLO) properties of synthesized complex were evaluated by the determining of dipole moment (µ), polarizability (α) and hyperpolarizability (β). Obtained results demonstrated that the manganese(II) complex is a good candidate for NLO material. Stability of the molecule arising from hyperconjugative interactions and charge delocalization was analyzed using natural bond orbital (NBO) analysis. The highest occupied and the lowest unoccupied molecular orbitals (HOMO and LUMO) which is also known the frontier molecular orbitals were simulated, and obtained energy gap confirmed that charge transfer occurs within manganese(II) complex. Molecular electrostatic potential (MEP) for synthesized manganese(II) complex displays the electrophilic and nucleophilic regions. From MEP, the the most negative region is located over carboxyl O atoms while positive region is located over H atoms.

Keywords: DFT, picolinate, IR, Raman, nonlinear optic

Procedia PDF Downloads 466

Authors: Samira Naghdi, Kyong Yop Rhee

Abstract:

Transfer-free synthesis of graphene on dielectric substrates is highly desirable but remains challenging. Here, by using a thin sacrificial platinum layer as a catalyst, graphene was deposited on a silicon substrate through a simple and transfer-free synthesis method. During graphene growth, the platinum layer evaporated, resulting in direct deposition of graphene on the silicon substrate. In this work, different growth conditions of graphene were optimized. Raman spectra of the produced graphene indicated that the obtained graphene was bilayer. The sheet resistance obtained from four-point probe measurements demonstrated that the deposited graphene had high conductivity. Reflectance spectroscopy of graphene-coated silicon showed a decrease in reflectance across the wavelength range of 200-800 nm, indicating that the graphene coating on the silicon surface had antireflection capabilities.

Keywords: antireflection coating, chemical vapor deposition, graphene, the sheet resistance

Procedia PDF Downloads 159

Authors: Eyob Belew Abebe

Abstract:

Nickel-rich layered oxide cathode materials having a Ni content of ≥ 90% have great potential for use in next-generation lithium-ion batteries (LIBs), due to their high energy densities and relatively low cost. They suffer, however, from poor cycling performance and rate capability, significantly hampering their widespread applicability. In this study we synthesized a Ni-rich precursor through a co-precipitation method and added different amounts of Li-excess on the precursors using a solid-state method to obtain sintered Li1+x(Ni0.9Co0.05Mn0.05)1–xO2 (denoted as L1+x-NCM; x = 0.00, 0.02, 0.04, 0.06, and 0.08) transition metal (TM) oxide cathode materials. The L1+x-NCM cathode having a Li-excess of 4% exhibited a discharge capacity of ca. 216.17 mAh g–1 at 2.7–4.3 V, 0.1C and retained 95.7% of its initial discharge capacity (ca. 181.39 mAh g–1) after 100 cycles of 1C charge/discharge which is the best performance as compared with stoichiometric Li1+x(Ni0.9Co0.05Mn0.05)1-xO2 (i.e. x=0, Li:TM = 1:1). Furthermore, a high-rate capability of ca. 162.92 mAh g–1 at a rate of 10C, led to the 4% Li-excess optimizing the electrochemical performance, relative to the other Li-excess samples. Ex/in-situ X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy revealed that the 4% Li-excess in the Ni-rich NCM90 cathode material: (i). decreased the Li+/Ni2+ disorder by increasing the content of Ni3+ in the TM slab, (ii). increased the crystallinity, and (iii). accelerated Li+ ion transport by widening the Li-slab. Furthermore, electrochemical impedance spectroscopy and cyclic voltammetry confirmed that the appropriate Li-excess lowered the electrochemical impedance and improved the reversibility of the electrochemical reaction. Therefore, our results revealed that NCM90 cathode materials featuring an optimal Li-excess are potential candidates for use in next-generation Li-ion batteries.

Keywords: LiNi₀.₉Co₀.₀₉Mn₀.₀₉O₂, li-excess, cation mixing, structure change, cycle stability, electrochemical properties

Procedia PDF Downloads 122

Authors: Subhojyoti Chatterjee, Peter J. Mahon, Feng Wang

Abstract:

Resveratrol (RvL), a phenolic compound, is a key ingredient in wine and tomatoes that has been studied over the years because of its important bioactivities such as anti-oxidant, anti-aging and antimicrobial properties. Out of the two isomeric forms of resveratrol i.e. trans and cis, the health benefit is primarily associated with the trans form. Thus, studying the structural properties of the isomers will not only provide an insight into understanding the RvL isomers, but will also help in designing parameters for differentiation in order to achieve 99.9% purity of trans-RvL. In the present study, density function theory (DFT) study is conducted, using the B3LYP/6-311++G** model to explore the through bond and through space intramolecular interactions. Properties such as vibrational spectroscopy (IR and Raman), nuclear magnetic resonance (NMR) spectra, excess orbital energy spectrum (EOES), energy based decomposition analyses (EDA) and Fukui function are calculated. It is discovered that the structure of trans-RvL, although it is C1 non-planar, the backbone non-H atoms are nearly in the same plane; whereas the cis-RvL consists of two major planes of R1 and R2 that are not in the same plane. The absence of planarity gives rise to a H-bond of 2.67Å in cis-RvL. Rotation of the C(5)-C(8) single bond in trans-RvL produces higher energy barriers since it may break the (planar) entire conjugated structure; while such rotation in cis-RvL produces multiple minima and maxima depending on the positions of the rings. The calculated FT-IR spectrum shows very different spectral features for trans and cis-RvL in the region 900 – 1500 cm-1, where the spectral peaks at 1138-1158 cm-1 are split in cis-RvL compared to a single peak at 1165 cm-1 in trans-RvL. In the Raman spectra, there is significant enhancement of cis-RvL in the region above 3000cm-1. Further, the carbon chemical environment (13C NMR) of the RvL molecule exhibit a larger chemical shift for cis-RvL compared to trans-RvL (Δδ = 8.18 ppm) for the carbon atom C(11), indicating that the chemical environment of the C group in cis-RvL is more diverse than its other isomer. The energy gap between highest occupied molecular orbital (HOMO) and the lowest occupied molecular orbital (LUMO) is 3.95 eV for trans and 4.35 eV for cis-RvL. A more detailed inspection using the recently developed EOES revealed that most of the large energy differences i.e. Δεcis-trans > ±0.30 eV, in their orbitals are contributed from the outer valence shell. They are MO60 (HOMO), MO52-55 and MO46. The active sites that has been captured by Fukui function (f + > 0.08) are associated with the stilbene C=C bond of RvL and cis-RvL is more active at these sites than in trans-RvL, as cis orientation breaks the large conjugation of trans-RvL so that the hydroxyl oxygen’s are more active in cis-RvL. Finally, EDA highlights the interaction energy (ΔEInt) of the phenolic compound, where trans is preferred over the cis-RvL (ΔΔEi = -4.35 kcal.mol-1) isomer. Thus, these quantum mechanics results could help in unwinding the diversified beneficial activities associated with resveratrol.

Keywords: resveratrol, FT-IR, Raman, NMR, excess orbital energy spectrum, energy decomposition analysis, Fukui function

Procedia PDF Downloads 172

Authors: Shivani A. Singh, Pravin S. More

Abstract:

In the present inspection, we indicate the falsification of Fe-doped graphene nanoparticles by modified Hummers method. Structural and physiochemical properties of the resulting pallets were explored with the help of ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), Photoluminescence spectroscopy (PL) for graphene sample exhibits absorption peaks ~248nm. Pure graphene shows PL peak at 348 nm. After doping of Fe with graphene the PL peak shifted from 348 nm to 332 nm. The oxidation degree, i.e. the relative amount of oxygen functional groups was estimated from the relative intensities of the oxygen related bands (ORB) in the FTIR measurements. These analyses show that this modified material can be useful for gas sensing applications and to be used in diverse areas.

Keywords: chemical doping, graphene, gas sensing, sensing

Procedia PDF Downloads 187

Authors: P. Tirgarbahnamiri, S. Mahravani, N. Haddadpour, F. Yaghmaie, F. Barazandeh

Abstract:

In this study, silver nanoparticle-Polydimethylsiloxane membrane (SNP-PDMS) was prepared with an in-situ reduction method using AgNO3 in poly (dimethylsiloxane) hardener. Optical and mechanical properties as well as functionality of these membranes were determined employing, UV-Vis spectrophotometry, FTIR, strain-stress test and liquid/liquid filtration measurements. Silver nanoparticles are known to selectively absorb Olefins and may be used for separation of Alkanes from olefins. Yellow color of silver nanocomposites and transparency of blank polymer were observed employing optical microscope. λmax in 415-420 nm regions in UV-Vis spectrophotometry are related to silver nanoparticles absorbance. Based on stress-strain test results, tensile strength of silver nanoparticle PDMS (SNP-PDMS) membranes is higher than PDMS films of comparable size and thickness. Moreover, permeability of SNP-PDMS membranes were characterized using similar olefin/paraffin pair using a simple bench scale separation set- up. The silver -PDMS membranes retain their color and UV-vis characteristics for extended periods of time exceeding several months.

Keywords: nanocomposite membrane, gas separation, facilitated transport, silver nanocomposite, PDMS, in-situ reduction

Procedia PDF Downloads 301

Authors: Miyeon Yoo, Sewon Kim, Changyeop Lee

Abstract:

It is important to measure the internal temperature or temperature distribution precisely in combustion system to increase energy efficiency and reduce the pollutants. Especially in case of large combustion systems such as power plant boiler and reheating furnace of steel making process, it is very difficult to measure those physical properties in detail. Tunable diode laser absorption spectroscopy measurement and analysis can be attractive method to overcome the difficulty. In this paper, TDLAS methods are used to measure the oxygen concentration and temperature distribution in various experimental conditions.

Keywords: tunable diode laser absorption Spectroscopy, temperature distribution, gas concentration

Procedia PDF Downloads 357

Authors: Pascal Mwenge, Tumisang Seodigeng

Abstract:

The combination of world population and the third industrial revolution led to high demand for fuels. On the other hand, the decrease of global fossil 8fuels deposits and the environmental air pollution caused by these fuels has compounded the challenges the world faces due to its need for energy. Therefore, new forms of environmentally friendly and renewable fuels such as biodiesel are needed. The primary analytical techniques for methanolysis yield monitoring have been chromatography and spectroscopy, these methods have been proven reliable but are more demanding, costly and do not provide real-time monitoring. In this work, the in situ monitoring of biodiesel from sunflower oil using FTIR (Fourier Transform Infrared) has been studied; the study was performed using EasyMax Mettler Toledo reactor equipped with a DiComp (Diamond) probe. The quantitative monitoring of methanolysis was performed by building a quantitative model with multivariate calibration using iC Quant module from iC IR 7.0 software. 15 samples of known concentrations were used for the modelling which were taken in duplicate for model calibration and cross-validation, data were pre-processed using mean centering and variance scale, spectrum math square root and solvent subtraction. These pre-processing methods improved the performance indexes from 7.98 to 0.0096, 11.2 to 3.41, 6.32 to 2.72, 0.9416 to 0.9999, RMSEC, RMSECV, RMSEP and R2Cum, respectively. The R² value of 1 (training), 0.9918 (test), 0.9946 (cross-validation) indicated the fitness of the model built. The model was tested against univariate model; small discrepancies were observed at low concentration due to unmodelled intermediates but were quite close at concentrations above 18%. The software eliminated the complexity of the Partial Least Square (PLS) chemometrics. It was concluded that the model obtained could be used to monitor methanol of sunflower oil at industrial and lab scale.

Keywords: biodiesel, calibration, chemometrics, methanolysis, multivariate analysis, transesterification, FTIR

Procedia PDF Downloads 126

Authors: N. Perini, M. C. Thaller, F. Mercuri, S. Orlanducci, A. Rubechini, L. Migliore

Abstract:

The preservation of cultural heritage is one of the major challenges of today’s society, because of the fundamental right of future generations to inherit it as the continuity with their historical and cultural identity. Parchments, consisting of a semi-solid matrix of collagen produced from animal skin (i.e., sheep or goats), are a significant part of the cultural heritage, being used as writing material for many centuries. Due to their animal origin, parchments easily undergo biodeterioration. The most common biological damage is characterized by isolated or coalescent purple spots that often leads to the detachment of the superficial layer and the loss of the written historical content of the document. Although many parchments with the same biodegradative features were analyzed, no common causative agent has been found so far. Very recently, a study was performed on a purple-damaged parchment roll dated back 1244 A.D, the A.A. Arm. I-XVIII 3328, belonging to the oldest collection of the Vatican Secret Archive (Fondo 'Archivum Arcis'), by comparing uncolored undamaged and purple damaged areas of the same document. As a whole, the study gave interesting results to hypothesize a model of biodeterioration, consisting of a microbial succession acting in two main phases: the first one, common to all the damaged parchments, is characterized by halophilic and halotolerant bacteria fostered by the salty environment within the parchment maybe induced by bringing of the hides; the second one, changing with the individual history of each parchment, determines the identity of its colonizers. The design of this model was pivotal to this study, performed by different labs of the Tor Vergata University (Rome, Italy), in collaboration with the Vatican Secret Archive. Three documents, belonging to a collection of dramatically damaged parchments archived as 'Faldone Patrizi A 19' (dated back XVII century A.D.), were analyzed through a multidisciplinary approach, including three updated technologies: (i) Next Generation Sequencing (NGS, Illumina) to describe the microbial communities colonizing the damaged and undamaged areas, (ii) RAMAN spectroscopy to analyze the purple pigments, (iii) Light Transmitted Analysis (LTA) to evaluate the kind and entity of the damage to native collagen. The metagenomic analysis obtained from NGS revealed DNA sequences belonging to Halobacterium salinarum mainly in the undamaged areas. RAMAN spectroscopy detected pigments within the purple spots, mainly bacteriorhodopsine/rhodopsin-like pigments, a purple transmembrane protein containing retinal and present in Halobacteria. The LTA technique revealed extremely damaged collagen structures in both damaged and undamaged areas of the parchments. In the light of these data, the study represents a first confirmation of the microbial succession model described above. The demonstration of this model is pivotal to start any possible new restoration strategy to bring back historical parchments to their original beauty, but also to open opportunities for intervention on a huge amount of documents.

Keywords: biodeterioration, parchments, purple spots, ecological succession

Procedia PDF Downloads 142

Authors: Samar Aoujia, Théo Guérineaub, Rayan Zaitera, Evelyne Fargina, Younès Messaddeqb, Thierry Cardinala

Abstract:

Two barium gallo-germanate glass series were elaborated to investigate the effect of the yttrium introduction on the glass physicochemical properties and crystallization behavior. One to twenty mol% of YO3/2 were either added into the glass matrix or substituted for gallium oxide. The glass structure was studied by Raman spectroscopy, and the thermal, optical, thermo-mechanical and physical properties are examined. The introduction of yttrium ions in both glass series increases the glass transition temperature, crystallization temperature, softening temperature, coefficient of linear thermal expansion and density. Through differential scanning calorimetry and X-ray diffraction analyses, it was found that competition occurs between the gallo-germanate zeolite-type phase and the yttrium-containing phase. From 13 mol% of YO3/2, the yttrium introduction impedes the formation of surface crystallization in these glasses.

Keywords: photonic, heavy-metal oxide, glass, crystallization

Procedia PDF Downloads 114

Authors: Noor-ul-Ain, Muhammad Tahir Khan, Kashif Khan, Adeela Ajmal, Hamid Mustafa

Abstract:

The objective of this study was to evaluate the preservative and upgrading potential of urea (70g/kg DM) added to high moisture oat silage at laboratory scale trial and urea was hydrolysed 95%. Microbial activity measured by pH and volatile fatty acids (VFA) and lactate production was reduced (p<0.001) by the urea addition. The pH of oat silage (without treated) was measured 5.7 and increased up to 8.00 on average while; volatile fatty acids (VFA) concentration was decreased. Relative proportions of fermentation acids changed after urea addition, increasing the acetate and butyrate and decreasing the propionate and lactate proportions. The addition of urea to oat silages increased (P<0.001) water soluble and ammonium nitrogen of the forage. These nitrogen fractions represented more than 40% of total nitrogen. After urea addition, total nitrogen content of oat silages increased from 21.0 g/kg DM to 28 g/kg DM. Application of urea at a rate of 70 g/kg DM significantly increased (P<0.001) the in situ degradation of neutral-detergent fibre after 48h of rumen incubation (NDF-situ). The NDF-situ was 200 g/kg NDF higher on oat forages ensiled with urea than on oat forages ensiled without urea. Oat silages can be effectively preserved and upgraded by ensiling with 70 g urea/kg dry matter. Further studies are required to evaluate voluntary intake of this forage.

Keywords: oat, silage, urea, pH, forage

Procedia PDF Downloads 443

Authors: Mohammad I. Hossain, Omar F. Hamim

Abstract:

This paper presents a case study on a pile integrity test for assessing the integrity of piles as well as a physical dimension (e.g., cross-sectional area, length), continuity, and consistency of the pile materials. The recent boom in the socio-economic condition of Bangladesh has given rise to the building of high-rise commercial and residential infrastructures. The advantage of the pile integrity test lies in the fact that it is possible to get an approximate indication regarding the quality of the sub-structure before commencing the construction of the super-structure. This paper aims at providing a classification of cast-in-situ piles based on characteristic reflectograms obtained using the Sonic Integrity Testing program for the sub-soil condition of Narayanganj, Bangladesh. The piles have been classified as 'Pile Type-1', 'Pile Type-2', 'Pile Type-3', 'Pile type-4', 'Pile Type-5' or 'Pile Type-6' from the visual observations of reflections from the generated stress waves by striking the pile head with a handheld hammer. With respect to construction quality and integrity, piles have been further classified into three distinct categories, i.e., satisfactory, may be satisfactory, and unsatisfactory.

Keywords: cast-in-situ piles, characteristic reflectograms, pile integrity test, sonic integrity testing program

Procedia PDF Downloads 93

Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

Abstract:

Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750 C analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry

Procedia PDF Downloads 527

Authors: J. V. Gonzalez Fernandez, T. Mozume, S. Gozu, A. Lastras Martinez, L. F. Lastras Martinez, J. Ortega Gallegos, R. E. Balderas Navarro

Abstract:

We report on a theoretical-experimental study of photoreflectance anisotropy (PRA) spectroscopy of coupled double quantum wells. By probing the in-plane interfacial optical anisotropies, we demonstrate that PRA spectroscopy has the capacity to detect and distinguish layers with quantum dimensions. In order to account for the experimental PRA spectra, we have used a theoretical model at k=0 based on a linear electro-optic effect through a piezoelectric shear strain.

Keywords: coupled double quantum well (CDQW), linear electro-optic (LEO) effect, photoreflectance anisotropy (PRA), piezoelectric shear strain

Procedia PDF Downloads 660

Authors: Ganesh R. Bhand, N. B. Chaure

Abstract:

Cadmium selenide (CdSe) quantum dots (QDs) were prepared by solvothermal route. Subsequently a inorganic QDs-organic semiconductor (copper phthalocyanine) nanocomposite (i.e CuPc:CdSe nanocomposites) were produced by different concentration of QDs varied in CuPc. The nanocomposite thin films have been prepared by means of spin coating technique. The optical, structural and morphological properties of nanocomposite films have been investigated. The transmission electron microscopy (TEM) confirmed the formation of QDs having average size of  4 nm. The X-ray diffraction pattern exhibits cubic crystal structure of CdSe with reflection to (111), (220) and (311) at 25.4ᵒ, 42.2ᵒ and 49.6ᵒ respectively. The additional peak observed at lower angle at 6.9ᵒ in nanocomposite thin films are associated to CuPc. The field emission scanning electron microscopy (FESEM) observed that surface morphology varied in increasing concentration of CdSe QDs. The obtained nanocomposite show significant improvement in the thermal stability as compared to the pure CuPc indicated by thermo-gravimetric analysis (TGA) in thermograph. The effect in the Raman spectra of composites samples gives a confirm evidence of homogenous dispersion of CdSe in the CuPc matrix and their strong interaction between them to promotes charge transfer property. The success of reaction between composite was confirmed by Fourier transform infrared spectroscopy (FTIR). The photo physical properties were studied using UV - visible spectroscopy. The enhancement of the optical absorption in visible region for nanocomposite layer was observed with increasing the concentration of CdSe in CuPc. This composite may obtain the maximized interface between QDs and polymer for efficient charge separation and enhance the charge transport. Such nanocomposite films for potential application in fabrication of hybrid solar cell with improved power conversion efficiency.

Keywords: CdSe QDs, cupper phthalocyanine, FTIR, optical absorption

Procedia PDF Downloads 176

Authors: M. G. Smitha, M. V. Murugendrappa

Abstract:

Perovskite manganite La_0.7Ca_0.3MnO₃ was synthesized by Sol-gel method. Polymerization of pyrrole was carried by in-situ polymerization method. The composite of pyrrole (Py)/La_0.7Ca_0.3MnO₃ composite in the presence of oxidizing agent ammonium per sulphate to synthesize polypyrrole (PPy)/La_0.7Ca_0.3MnO₃ (LCM) composite was carried out by the same in-situ polymerization method. The PPy/LCM composites were synthesized with varying compositions like 10, 20, 30, 40, and 50 wt.% of LCM in Py. The surface morphologies of these composites were analyzed by using scanning electron microscope (SEM). The images show that LCM particles are embedded in PPy chain. The impedance measurement of PPy/LCM at different temperature ranges from 30 to 180 °C was studied using impedance analyzer. The study shows that impedance is frequency and temperature dependent and it is found to decrease with increase in frequency and temperature.

Keywords: polypyrrole, sol gel, impedance, composites

Procedia PDF Downloads 351

Authors: Rajinder Kaur, Atul Khanna

Abstract:

Transparent glass-ceramic and crystalline samples of the system: xSrO-(100-x)TeO2; x = 7.5 and 8.5 mol% were prepared by quenching the melts in the temperature range of 700 to 950oC. A very interesting effect of the temperature on the glass-forming ability (GFA) of strontium tellurite melts is observed,and it is found that the melts produce transparent glass-ceramics when it is solidified from lower temperatures in the range of 700-750oC, however, when the melts are cooled from higher temperatures in the range of 850-950oC, the GFA is significantly reduced andanti-glass and/or crystalline phases are produced on solidification.The effect of temperature on GFA of strontium tellurite melts is attributed to short-range structural transformations: TeO₄TeO₃ which procceds towards the right side with an increrase in temperature. This isomerization reaction lowers the melt viscosity and enhances the crystallization tedendency. It is concluded that the high-temperature strontium tellurite meltsfreeze faster into crystalline phases as compared to the melts at a lower temperature; the latter supercooland solidify into glassy phases.

Keywords: anti-glasss, ceramic, supercool liquid, raman spectroscopy

Procedia PDF Downloads 49

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

Abstract:

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

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

Procedia PDF Downloads 121

Authors: Ali Mortazavi

Abstract:

The main objective of this research project is to delve into a multitude of geomechanical risks associated with various mining methods employed within the underground mining industry. Controlling geotechnical design parameters and operational factors affecting the selection of suitable mining techniques for a given underground mining condition will be considered from a risk assessment point of view. Important geomechanical challenges will be investigated as appropriate and relevant to the commonly used underground mining methods. Given the complicated nature of rock mass in-situ and complicated boundary conditions and operational complexities associated with various underground mining methods, the selection of a safe and economic mining operation is of paramount significance. Rock failure at varying scales within the underground mining openings is always a threat to mining operations and causes human and capital losses worldwide. Geotechnical design is a major design component of all underground mines and basically dominates the safety of an underground mine. With regard to uncertainties that exist in rock characterization prior to mine development, there are always risks associated with inappropriate design as a function of mining conditions and the selected mining method. Uncertainty often results from the inherent variability of rock masse, which in turn is a function of both geological materials and rock mass in-situ conditions. The focus of this research is on developing a methodology which enables a geomechanical risk assessment of given underground mining conditions. The outcome of this research is a geotechnical risk analysis algorithm, which can be used as an aid in selecting the appropriate mining method as a function of mine design parameters (e.g., rock in-situ properties, design method, governing boundary conditions such as in-situ stress and groundwater, etc.).

Keywords: geomechanical risk assessment, rock mechanics, underground mining, rock engineering

Procedia PDF Downloads 115

Authors: Xie Xiaobin, Zhang Yan, Shi Yipeng, Sun Wenying, Chen Shuang, Cai Zhipeng, Zhang Hong, Zhang Lixia, Xie Like

Abstract:

Objective: The objective of this research is to compare the efficacy of the late in-situ surgical revision augmented with continuous infusion and needle revision on failed trabeculectomy blebs. Methods From December 2018 to December 2021, a prospective randomized controlled trial was performed on 44 glaucoma patients with failed bleb ≥ 6months with medically uncontrolled in Eye Hospital, China Academy of Chinese Medical Sciences. They were randomly divided into two groups. 22 eyes of 22 patients underwent the late in-situ surgical revision with continuous anterior chamber infusion in the study group, and 22 of 22 patients were treated with needle revision in the control group. Main outcome measures include preoperative and postoperative intraocular pressure (IOP), the number of anti-glaucoma medicines, the operation success rate, and the postoperative complications. Results The postoperative IOP values decreased significantly from the baseline in both groups (both P<0.05). IOP was significantly lower in the study group than in the control group at one week, 1, and 3 months postoperatively (all P<0.05). IOP reductions in the study group were substantially more prominent than in the control group at all postoperative time points (all P<0.05). The complete success rate in the study group was significantly higher than in the control group (71.4% vs. 33.3%, P<0.05), while the complete failure rate was significantly lower in the study group (0% vs. 28.5%, P<0.05). According to Cox’s proportional hazards regression analysis, high IOP at baseline was independently associated with increased risks of complete failure (adjusted hazard ratio=1.141, 95% confidence interval=1.021-1.276, P<0.05). There was no significant difference in the incidence of postoperative complications between the two groups (P>0.05). Conclusion: Both in-situ surgical and needle revision have acceptable success rates and safety for the late failed trabeculectomy blebs, while the former is likely to have a higher level of efficacy over the latter. Needle revision may be insufficient for eyes with low target IOP.

Keywords: glaucoma, trabeculectomy blebs, in-situ surgical revision, needle revision

Procedia PDF Downloads 65

Authors: M. A. Karakassides, M. Baikousi, A. Kouloumpis, D. Gournis

Abstract:

Nanocomposites of Carbon Nanorods (CNRs) with Polystyrene (PS), have been synthesized successfully by means of in situ polymerization process and characterized. Firstly, carbon nanorods with graphitic structure were prepared by the standard synthetic procedure of CMK-3 using MCM-41 as template, instead of SBA-15, and sucrose as carbon source. In order to create an organophilic surface on CNRs, two parts of modification were realized: surface chemical oxidation (CNRs-ox) according to the Staudenmaier’s method and the attachment of octadecylamine molecules on the functional groups of CNRs-ox (CNRs-ODA The nanocomposite materials of polystyrene with CNRs-ODA, were prepared by a solution-precipitation method at three nanoadditive to polymer loadings (1, 3 and 5 wt. %). The as derived nanocomposites were studied with a combination of characterization and analytical techniques. Especially, Fourier-transform infrared (FT-IR) and Raman spectroscopies were used for the chemical and structural characterization of the pristine materials and the derived nanocomposites while the morphology of nanocomposites and the dispersion of the carbon nanorods were analyzed by atomic force and scanning electron microscopy techniques. Tensile testing and thermogravimetric analysis (TGA) along with differential scanning calorimetry (DSC) were also used to examine the mechanical properties and thermal stability -glass transition temperature of PS after the incorporation of CNRs-ODA nanorods. The results showed that the thermal and mechanical properties of the PS/ CNRs-ODA nanocomposites gradually improved with increasing of CNRs-ODA loading.

Keywords: nanocomposites, polystyrene, carbon, nanorods

Procedia PDF Downloads 322