Search results for: in-situ laser raman spectroscopy
1717 Temperature Dependence of Photoluminescence Intensity of Europium Dinuclear Complex
Authors: Kwedi L. M. Nsah, Hisao Uchiki
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Quantum computation is a new and exciting field making use of quantum mechanical phenomena. In classical computers, information is represented as bits, with values either 0 or 1, but a quantum computer uses quantum bits in an arbitrary superposition of 0 and 1, enabling it to reach beyond the limits predicted by classical information theory. lanthanide ion quantum computer is an organic crystal, having a lanthanide ion. Europium is a favored lanthanide, since it exhibits nuclear spin coherence times, and Eu(III) is photo-stable and has two stable isotopes. In a europium organic crystal, the key factor is the mutual dipole-dipole interaction between two europium atoms. Crystals of the complex were formed by making a 2 :1 reaction of Eu(fod)3 and bpm. The transparent white crystals formed showed brilliant red luminescence with a 405 nm laser. The photoluminescence spectroscopy was observed both at room and cryogenic temperatures (300-14 K). The luminescence spectrum of [Eu(fod)3(μ-bpm) Eu(fod)3] showed characteristic of Eu(III) emission transitions in the range 570–630 nm, due to the deactivation of 5D0 emissive state to 7Fj. For the application of dinuclear Eu3+ complex to q-bit device, attention was focused on 5D0 -7F0 transition, around 580 nm. The presence of 5D0 -7F0 transition at room temperature revealed that at least one europium symmetry had no inversion center. Since the line was unsplit by the crystal field effect, any multiplicity observed was due to a multiplicity of Eu3+ sites. For q-bit element, more narrow line width of 5D0 → 7F0 PL band in Eu3+ ion was preferable. Cryogenic temperatures (300 K – 14 K) was applicable to reduce inhomogeneous broadening and distinguish between ions. A CCD image sensor was used for low temperature Photoluminescence measurement, and a far better resolved luminescent spectrum was gotten by cooling the complex at 14 K. A red shift by 15 cm-1 in the 5D0 - 7F0 peak position was observed upon cooling, the line shifted towards lower wavenumber. An emission spectrum at the 5D0 - 7F0 transition region was obtained to verify the line width. At this temperature, a peak with magnitude three times that at room temperature was observed. The temperature change of the 5D0 state of Eu(fod)3(μ-bpm)Eu(fod)3 showed a strong dependence in the vicinity of 60 K to 100 K. Thermal quenching was observed at higher temperatures than 100 K, at which point it began to decrease slowly with increasing temperature. The temperature quenching effect of Eu3+ with increase temperature was caused by energy migration. 100 K was the appropriate temperature for the observation of the 5D0 - 7F0 emission peak. Europium dinuclear complex bridged by bpm was successfully prepared and monitored at cryogenic temperatures. At 100 K the Eu3+-dope complex has a good thermal stability and this temperature is appropriate for the observation of the 5D0 - 7F0 emission peak. Sintering the sample above 600o C could also be a method to consider but the Eu3+ ion can be reduced to Eu2+, reasons why cryogenic temperature measurement is preferably over other methods.Keywords: Eu(fod)₃, europium dinuclear complex, europium ion, quantum bit, quantum computer, 2, 2-bipyrimidine
Procedia PDF Downloads 1811716 Linking Soil Spectral Behavior and Moisture Content for Soil Moisture Content Retrieval at Field Scale
Authors: Yonwaba Atyosi, Moses Cho, Abel Ramoelo, Nobuhle Majozi, Cecilia Masemola, Yoliswa Mkhize
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Spectroscopy has been widely used to understand the hyperspectral remote sensing of soils. Accurate and efficient measurement of soil moisture is essential for precision agriculture. The aim of this study was to understand the spectral behavior of soil at different soil water content levels and identify the significant spectral bands for soil moisture content retrieval at field-scale. The study consisted of 60 soil samples from a maize farm, divided into four different treatments representing different moisture levels. Spectral signatures were measured for each sample in laboratory under artificial light using an Analytical Spectral Device (ASD) spectrometer, covering a wavelength range from 350 nm to 2500 nm, with a spectral resolution of 1 nm. The results showed that the absorption features at 1450 nm, 1900 nm, and 2200 nm were particularly sensitive to soil moisture content and exhibited strong correlations with the water content levels. Continuum removal was developed in the R programming language to enhance the absorption features of soil moisture and to precisely understand its spectral behavior at different water content levels. Statistical analysis using partial least squares regression (PLSR) models were performed to quantify the correlation between the spectral bands and soil moisture content. This study provides insights into the spectral behavior of soil at different water content levels and identifies the significant spectral bands for soil moisture content retrieval. The findings highlight the potential of spectroscopy for non-destructive and rapid soil moisture measurement, which can be applied to various fields such as precision agriculture, hydrology, and environmental monitoring. However, it is important to note that the spectral behavior of soil can be influenced by various factors such as soil type, texture, and organic matter content, and caution should be taken when applying the results to other soil systems. The results of this study showed a good agreement between measured and predicted values of Soil Moisture Content with high R2 and low root mean square error (RMSE) values. Model validation using independent data was satisfactory for all the studied soil samples. The results has significant implications for developing high-resolution and precise field-scale soil moisture retrieval models. These models can be used to understand the spatial and temporal variation of soil moisture content in agricultural fields, which is essential for managing irrigation and optimizing crop yield.Keywords: soil moisture content retrieval, precision agriculture, continuum removal, remote sensing, machine learning, spectroscopy
Procedia PDF Downloads 991715 Rapid Green Synthesis of Silver Nanoparticles Using Solanum Nigrum Leaves Extract with Antimicrobial and Anticancer Properties
Authors: Anushaa A.
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In this work, silver nanoparticles (AgNP) were manufactured directly without harmful chemicals utilising methanol extract (SNLME) Solanum nigrume leaves. We are using nigrum leaf extract from Solanum, which converts silver nitrate to silver ions, for synthesization purposes. An examination of the AgNP produced was performed using ultraviolet (UV-VIS) spectroscopy, infrared spectroscopy (FTIR) transformed from Fourier and scanning electrons (SEM). Biological activity was also tested. UV-VIS has proven that biosynthesized AgNP exists (420-450 nm). The FTIR spectrum has been utilised to confirm the presence of different functional groups within the biomolecules, which are a nanoparticular capping agent and the spectroscopic and crystal nature of AgNP. The viability of the silver nanoparticles was evaluated using zeta potential calculations. Negative zeta potential of -33.4 mV demonstrated the stability of silver-nanoparticles. The morphology of AgNP was examined using a scanning electron microscope. Greenly generated AgNP showed significant anti-Staphylococcus aureus, Candida, and Escherichia coli action. The green AgNP demonstration indicated that the IC50 for the human teratocarcinoma cell line was 29.24 μg/ml during 24 hours of therapy (PA1 Ovarian cell line). The dose-dependent effects were reported in both antibacterial and cytotoxicity assays and as an effective agent. Finally, the findings of this research showed that silver nanoparticles generated might serve as a viable therapeutic agent to combat microorganisms killing and curing cancer.Keywords: antimicrobial activity, PA1 ovarian cancer cell line, silver nanoparticles, Solanum nigrum
Procedia PDF Downloads 1871714 Application of Neutron Stimulated Gamma Spectroscopy for Soil Elemental Analysis and Mapping
Authors: Aleksandr Kavetskiy, Galina Yakubova, Nikolay Sargsyan, Stephen A. Prior, H. Allen Torbert
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Determining soil elemental content and distribution (mapping) within a field are key features of modern agricultural practice. While traditional chemical analysis is a time consuming and labor-intensive multi-step process (e.g., sample collections, transport to laboratory, physical preparations, and chemical analysis), neutron-gamma soil analysis can be performed in-situ. This analysis is based on the registration of gamma rays issued from nuclei upon interaction with neutrons. Soil elements such as Si, C, Fe, O, Al, K, and H (moisture) can be assessed with this method. Data received from analysis can be directly used for creating soil elemental distribution maps (based on ArcGIS software) suitable for agricultural purposes. The neutron-gamma analysis system developed for field application consisted of an MP320 Neutron Generator (Thermo Fisher Scientific, Inc.), 3 sodium iodide gamma detectors (SCIONIX, Inc.) with a total volume of 7 liters, 'split electronics' (XIA, LLC), a power system, and an operational computer. Paired with GPS, this system can be used in the scanning mode to acquire gamma spectra while traversing a field. Using acquired spectra, soil elemental content can be calculated. These data can be combined with geographical coordinates in a geographical information system (i.e., ArcGIS) to produce elemental distribution maps suitable for agricultural purposes. Special software has been developed that will acquire gamma spectra, process and sort data, calculate soil elemental content, and combine these data with measured geographic coordinates to create soil elemental distribution maps. For example, 5.5 hours was needed to acquire necessary data for creating a carbon distribution map of an 8.5 ha field. This paper will briefly describe the physics behind the neutron gamma analysis method, physical construction the measurement system, and main characteristics and modes of work when conducting field surveys. Soil elemental distribution maps resulting from field surveys will be presented. and discussed. Comparison of these maps with maps created on the bases of chemical analysis and soil moisture measurements determined by soil electrical conductivity was similar. The maps created by neutron-gamma analysis were reproducible, as well. Based on these facts, it can be asserted that neutron stimulated soil gamma spectroscopy paired with GPS system is fully applicable for soil elemental agricultural field mapping.Keywords: ArcGIS mapping, neutron gamma analysis, soil elemental content, soil gamma spectroscopy
Procedia PDF Downloads 1341713 Experimental Damping Performance of Composite Materials with Different Fibre Orientations
Authors: Ferhat Kadioglu
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A clamped-free vibrating beam technique was used to evaluate dynamic properties of glass fiber reinforced polymer matrix composite. In the experiment, an electromagnetic shaker and a non-contact laser head were used to vibrate and to take the response of the specimens, respectively. Test results showed that damping and elastic modulus of the material, as dynamic properties, could be obtained successfully using this technique. It was found that the balanced and symmetric specimens with 45 degrees are the best for damping performance. It is believed that such results could be used for the modal design of aerospace structures.Keywords: composite materials, damping values, dynamic properties, non-contact measurements
Procedia PDF Downloads 3481712 Using MALDI-TOF MS to Detect Environmental Microplastics (Polyethylene, Polyethylene Terephthalate, and Polystyrene) within a Simulated Tissue Sample
Authors: Kara J. Coffman-Rea, Karen E. Samonds
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Microplastic pollution is an urgent global threat to our planet and human health. Microplastic particles have been detected within our food, water, and atmosphere, and found within the human stool, placenta, and lung tissue. However, most spectrometric microplastic detection methods require chemical digestion which can alter or destroy microplastic particles and makes it impossible to acquire information about their in-situ distribution. MALDI TOF MS (Matrix-assisted laser desorption ionization-time of flight mass spectrometry) is an analytical method using a soft ionization technique that can be used for polymer analysis. This method provides a valuable opportunity to both acquire information regarding the in-situ distribution of microplastics and also minimizes the destructive element of chemical digestion. In addition, MALDI TOF MS allows for expanded analysis of the microplastics including detection of specific additives that may be present within them. MALDI TOF MS is particularly sensitive to sample preparation and has not yet been used to analyze environmental microplastics within their specific location (e.g., biological tissues, sediment, water). In this study, microplastics were created using polyethylene gloves, polystyrene micro-foam, and polyethylene terephthalate cable sleeving. Plastics were frozen using liquid nitrogen and ground to obtain small fragments. An artificial tissue was created using a cellulose sponge as scaffolding coated with a MaxGel Extracellular Matrix to simulate human lung tissue. Optimal preparation techniques (e.g., matrix, cationization reagent, solvent, mixing ratio, laser intensity) were first established for each specific polymer type. The artificial tissue sample was subsequently spiked with microplastics, and specific polymers were detected using MALDI-TOF-MS. This study presents a novel method for the detection of environmental polyethylene, polyethylene terephthalate, and polystyrene microplastics within a complex sample. Results of this study provide an effective method that can be used in future microplastics research and can aid in determining the potential threats to environmental and human health that they pose.Keywords: environmental plastic pollution, MALDI-TOF MS, microplastics, polymer identification
Procedia PDF Downloads 2561711 Dy3+ Ions Doped Single and Mixed Alkali Fluoro Tungstunate Tellurite Glasses for Laser and White LED Applications
Authors: Allam Srinivasa Rao, Ch. Annapurna Devi, G. Vijaya Prakash
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A new-fangled series of white light emitting 1 mol% of Dy3+ ions doped Single-Alklai and Mixed-Alkai fluoro tungstunate tellurite glasses have been prepared using melt quenching technique and their spectroscopic behaviour was investigated by studying XRD, optical absorption, photoluminescence and lifetime measurements. The bonding parameter studies reveal the ionic nature of the Dy-O bond in the present glasses. From the absorption spectra, the Judd–Ofelt (J-O) intensity parameters have been determined which are used to explore the nature of bonding and symmetry orientation of the Dy–ligand field environment. The evaluated J-O parameters (Ω_4>Ω_2>Ω_6) for all the glasses are following the same trend. The photoluminescence spectra of all the glasses exhibit two intensified peaks in blue and Yellow regions corresponding to the transitions 4F9/2→6H15/2 (483 nm) and 4F9/2→6H13/2 (575 nm) respectively. From the photoluminescence spectra, it is observed that the luminescence intensity is maximum for Dy3+ ion doped potassium combination of fluoro tungstunate tellurite glass (TeWK: 1Dy). The J-O intensity parameters have been used to determine the various radiative properties for the different emission transitions from the 4F9/2 fluorescent level. The highest emission cross-section and branching ratio values observed for the 4F9/2→6H15/2 and 4F9/2→6H13/2 transitions suggest the possible laser action in the visible region from these glasses. By using the experimental lifetimes (τ_exp) measured from the decay spectral features and radiative lifetimes (τ_R), the quantum efficiencies (η) for all the glasses have been evaluated. Among all the glasses, the potassium combined fluoro tungstunate tellurite (TeWK:1Dy) glass has the highest quantum efficiency (94.6%). The CIE colour chromaticity coordinates (x, y), (u, v), colour correlated temperature (CCT) and Y/B ratio were also estimated from the photoluminescence spectra for different compositions of glasses. The (x, y) and (u, v) chromaticity colour coordinates fall within the white light region and the white light can be tuned by varying the composition of the glass. From all these studies, we are suggesting that the 1 mol% of Dy3+ ions doped TeWK glass is more suitable for lasing and White-LED applications.Keywords: dysprosium, Judd-Ofelt parameters, photo luminescence, tellurite glasses
Procedia PDF Downloads 2241710 Design of a Portable Shielding System for a Newly Installed NaI(Tl) Detector
Authors: Mayesha Tahsin, A.S. Mollah
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Recently, a 1.5x1.5 inch NaI(Tl) detector based gamma-ray spectroscopy system has been installed in the laboratory of the Nuclear Science and Engineering Department of the Military Institute of Science and Technology for radioactivity detection purposes. The newly installed NaI(Tl) detector has a circular lead shield of 22 mm width. An important consideration of any gamma-ray spectroscopy is the minimization of natural background radiation not originating from the radioactive sample that is being measured. Natural background gamma-ray radiation comes from naturally occurring or man-made radionuclides in the environment or from cosmic sources. Moreover, the main problem with this system is that it is not suitable for measurements of radioactivity with a large sample container like Petridish or Marinelli beaker geometry. When any laboratory installs a new detector or/and new shield, it “must” first carry out quality and performance tests for the detector and shield. This paper describes a new portable shielding system with lead that can reduce the background radiation. Intensity of gamma radiation after passing the shielding will be calculated using shielding equation I=Ioe-µx where Io is initial intensity of the gamma source, I is intensity after passing through the shield, µ is linear attenuation coefficient of the shielding material, and x is the thickness of the shielding material. The height and width of the shielding will be selected in order to accommodate the large sample container. The detector will be surrounded by a 4π-geometry low activity lead shield. An additional 1.5 mm thick shield of tin and 1 mm thick shield of copper covering the inner part of the lead shielding will be added in order to remove the presence of characteristic X-rays from the lead shield.Keywords: shield, NaI (Tl) detector, gamma radiation, intensity, linear attenuation coefficient
Procedia PDF Downloads 1591709 Design and Development of Graphene Oxide Modified by Chitosan Nanosheets Showing pH-Sensitive Surface as a Smart Drug Delivery System for Control Release of Doxorubicin
Authors: Parisa Shirzadeh
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Drug delivery systems in which drugs are traditionally used, multi-stage and at specified intervals by patients, do not meet the needs of the world's up-to-date drug delivery. In today's world, we are dealing with a huge number of recombinant peptide and protean drugs and analogues of hormones in the body, most of which are made with genetic engineering techniques. Most of these drugs are used to treat critical diseases such as cancer. Due to the limitations of the traditional method, researchers sought to find ways to solve the problems of the traditional method to a large extent. Following these efforts, controlled drug release systems were introduced, which have many advantages. Using controlled release of the drug in the body, the concentration of the drug is kept at a certain level, and in a short time, it is done at a higher rate. Graphene is a natural material that is biodegradable, non-toxic, and natural compared to carbon nanotubes; its price is lower than carbon nanotubes and is cost-effective for industrialization. On the other hand, the presence of highly effective surfaces and wide surfaces of graphene plates makes it more effective to modify graphene than carbon nanotubes. Graphene oxide is often synthesized using concentrated oxidizers such as sulfuric acid, nitric acid, and potassium permanganate based on Hummer 1 method. In comparison with the initial graphene, the resulting graphene oxide is heavier and has carboxyl, hydroxyl, and epoxy groups. Therefore, graphene oxide is very hydrophilic and easily dissolves in water and creates a stable solution. On the other hand, because the hydroxyl, carboxyl, and epoxy groups created on the surface are highly reactive, they have the ability to work with other functional groups such as amines, esters, polymers, etc. Connect and bring new features to the surface of graphene. In fact, it can be concluded that the creation of hydroxyl groups, Carboxyl, and epoxy and in fact graphene oxidation is the first step and step in creating other functional groups on the surface of graphene. Chitosan is a natural polymer and does not cause toxicity in the body. Due to its chemical structure and having OH and NH groups, it is suitable for binding to graphene oxide and increasing its solubility in aqueous solutions. Graphene oxide (GO) has been modified by chitosan (CS) covalently, developed for control release of doxorubicin (DOX). In this study, GO is produced by the hummer method under acidic conditions. Then, it is chlorinated by oxalyl chloride to increase its reactivity against amine. After that, in the presence of chitosan, the amino reaction was performed to form amide transplantation, and the doxorubicin was connected to the carrier surface by π-π interaction in buffer phosphate. GO, GO-CS, and GO-CS-DOX characterized by FT-IR, RAMAN, TGA, and SEM. The ability to load and release is determined by UV-Visible spectroscopy. The loading result showed a high capacity of DOX absorption (99%) and pH dependence identified as a result of DOX release from GO-CS nanosheet at pH 5.3 and 7.4, which show a fast release rate in acidic conditions.Keywords: graphene oxide, chitosan, nanosheet, controlled drug release, doxorubicin
Procedia PDF Downloads 1201708 Deciphering Electrochemical and Optical Properties of Folic Acid for the Applications of Tissue Engineering and Biofuel Cell
Authors: Sharda Nara, Bansi Dhar Malhotra
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Investigation of the vitamins as an electron transfer mediator could significantly assist in merging the area of tissue engineering and electronics required for the implantable therapeutic devices. The present study report that the molecules of folic acid released by Providencia rettgeri via fermentation route under the anoxic condition of the microbial fuel cell (MFC) exhibit characteristic electrochemical and optical properties, as indicated by absorption spectroscopy, photoluminescence (PL), and cyclic voltammetry studies. The absorption spectroscopy has depicted an absorption peak at 263 nm with a small bulge around 293 nm on day two of bacterial culture, whereas an additional peak was observed at 365 nm on the twentieth day. Furthermore, the PL spectra has indicated that the maximum emission occurred at various wavelengths 420, 425, 440, and 445 nm when excited by 310, 325, 350, and 365 nm. The change of emission spectra with varying excitation wavelength might be indicating the presence of tunable optical bands in the folic acid molecules co-related with the redox activity of the molecules. The results of cyclic voltammetry studies revealed that the oxidation and reduction occurred at 0.25V and 0.12V, respectively, indicating the electrochemical behavior of the folic acid. This could be inferred that the released folic acid molecules in a MFC might undergo inter as well as intra molecular electron transfer forming different intermediate states while transferring electrons to the electrode surface. Synchronization of electrochemical and optical properties of folic acid molecules could be potentially promising for the designing of electroactive scaffold and biocompatible conductive surface for the applications of tissue engineering and biofuel cells, respectively.Keywords: biofuel cell, electroactivity, folic acid, tissue engineering
Procedia PDF Downloads 1311707 Research on the Effect of Coal Ash Slag Structure Evolution on Its Flow Behavior During Co-gasification of Coal and Indirect Coal Liquefaction Residue
Authors: Linmin Zhang
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Entrained-flow gasification technology is considered the most promising gasification technology because of its clean and efficient utilization characteristics. The stable fluidity of slag at high temperatures is the key to affecting the long-period operation of the gasifier. The diversity and differences of coal ash-slag systems make it difficult to meet the requirements for stable slagging in entrained-flow gasifiers. Therefore, coal blending or adding fluxes has been used in industry for a long time to improve the flow behavior of coal ash. As a by-product of the indirect coal liquefaction process, indirect coal liquefaction residue (ICLR) is a kind of industrial solid waste that is usually disposed of by stacking or landfilling. However, this disposal method will not only occupy land resources but also cause serious pollution to soil and water bodies by leachate containing toxic and harmful metals. As a carbon-containing matrix, ICLR is not only a kind of waste but also a kind of energy substance. Utilizing existing industrial gasifiers to blend combustion ICLR can not only transform industrial solid waste into fuel but also save coal resources. Moreover, the ICLR usually contains a unique ash chemical composition different from coal, which will affect the slagging performance of the gasifier. Therefore, exploring the effect of the ash addition in ICLR on the coal ash flow behavior can not only improve the slagging performance and gasification efficiency of entrained-flow gasifier by using the unique ash chemical composition of ICLR but also provide some theoretical support for the large-scale consumption of industrial solid waste. Combining molecular dynamics simulation with Raman spectroscopy experiment, the effect of ICLR addition on slag structure and fluidity was explained, and the relationship between the evolution law of slag short/medium range microstructure and macroscopic flow behavior was discussed. The research found that the high silicon and aluminum content in coal ash led to the formation of complex [SiO₄]⁴- tetrahedron and [AlO₄]⁵- tetrahedron structures at high temperature, and the [SiO₄]⁴- tetrahedron and [AlO₄]⁵- tetrahedron were connected by oxygen atoms to form a multi-membered ring structure with high polymerization degree. Due to the action of the multi-membered ring structure, the internal friction in the slag increased, and the viscosity value was higher on the macro-level. As a network-modified ion, Fe2+ could replace Si4+ and Al3+ in the multi-membered ring structure and combine with O2-, which will destroy the bridge oxygen (BO) structure and transform more complex tri cluster oxygen (TO) and bridge oxygen (BO) into simple non-bridge oxygen (NBO) structure. As a result, a large number of multi-membered rings with high polymerization degrees were depolymerized into low-membered rings with low polymerization degrees. The evolution of oxygen types and ring structures in slag reduced the structure complexity and polymerization degree of coal ash slag, resulting in a decrease in the viscosity of coal ash slag.Keywords: ash slag, coal gasification, fluidity, industrial solid waste, slag structure
Procedia PDF Downloads 301706 Photoswitchable and Polar-Dependent Fluorescence of Diarylethenes
Authors: Sofia Lazareva, Artem Smolentsev
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Fluorescent photochromic materials collect strong interest due to their possible application in organic photonics such as optical logic systems, optical memory, visualizing sensors, as well as characterization of polymers and biological systems. In photochromic fluorescence switching systems the emission of fluorophore is modulated between ‘on’ and ‘off’ via the photoisomerization of photochromic moieties resulting in effective resonance energy transfer (FRET). In current work, we have studied both photochromic and fluorescent properties of several diarylethenes. It was found that coloured forms of these compounds are not fluorescent because of the efficient intramolecular energy transfer. Spectral and photochromic parameters of investigated substances have been measured in five solvents having different polarity. Quantum yields of photochromic transformation A↔B ΦA→B and ΦB→A as well as B isomer extinction coefficients were determined by kinetic method. It was found that the photocyclization reaction quantum yield of all compounds decreases with the increase of solvent polarity. In addition, the solvent polarity is revealed to affect fluorescence significantly. Increasing of the solvent dielectric constant was found to result in a strong shift of emission band position from 450 nm (nhexane) to 550 nm (DMSO and ethanol) for all three compounds. Moreover, the emission intensive in polar solvents becomes weak and hardly detectable in n-hexane. The only one exception in the described dependence is abnormally low fluorescence quantum yield in ethanol presumably caused by the loss of electron-donating properties of nitrogen atom due to the protonation. An effect of the protonation was also confirmed by the addition of concentrated HCl in solution resulting in a complete disappearance of the fluorescent band. Excited state dynamics were investigated by ultrafast optical spectroscopy methods. Kinetic curves of excited states absorption and fluorescence decays were measured. Lifetimes of transient states were calculated from the data measured. The mechanism of ring opening reaction was found to be polarity dependent. Comparative analysis of kinetics measured in acetonitrile and hexane reveals differences in relaxation dynamics after the laser pulse. The most important fact is the presence of two decay processes in acetonitrile, whereas only one is present in hexane. This fact supports an assumption made on the basis of steady-state preliminary experiments that in polar solvents occur stabilization of TICT state. Thus, results achieved prove the hypothesis of two channel mechanism of energy relaxation of compounds studied.Keywords: diarylethenes, fluorescence switching, FRET, photochromism, TICT state
Procedia PDF Downloads 6791705 Preliminary Evaluation of Echinacea Species by UV-VIS Spectroscopy Fingerprinting of Phenolic Compounds
Authors: Elena Ionescu, Elena Iacob, Marie-Louise Ionescu, Carmen Elena Tebrencu, Oana Teodora Ciuperca
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Echinacea species (Asteraceae) has received a global attention because it is widely used for treatment of cold, flu and upper respiratory tract infections. Echinacea species contain a great variety of chemical components that contribute to their activity. The most important components responsible for the biological activity are those with high molecular-weight such as polysaccharides, polyacetylenes, highly unsaturated alkamides and caffeic acid derivatives. The principal factors that may influence the chemical composition of Echinacea include the species and the part of plant used (aerial parts or roots ). In recent years the market for Echinacea has grown rapidly and also the cases of adultery/replacement especially for Echinacea root. The identification of presence or absence of same biomarkers provide information for safe use of Echinacea species in food supplements industry. The aim of the study was the preliminary evaluation and fingerprinting by UV-VISIBLE spectroscopy of biomarkers in terms of content in phenolic derivatives of some Echinacea species (E. purpurea, E. angustifolia and E. pallida) for identification and authentication of the species. The steps of the study were: (1) samples (extracts) preparation from Echinacea species (non-hydrolyzed and hydrolyzed ethanol extracts); (2) samples preparation of reference substances (polyphenol acids: caftaric acid, caffeic acid, chlorogenic acid, ferulic acid; flavonoids: rutoside, hyperoside, isoquercitrin and their aglycones: quercitri, quercetol, luteolin, kaempferol and apigenin); (3) identification of specific absorption at wavelengths between 700-200 nm; (4) identify the phenolic compounds from Echinacea species based on spectral characteristics and the specific absorption; each class of compounds corresponds to a maximum absorption in the UV spectrum. The phytochemical compounds were identified at specific wavelengths between 700-200 nm. The absorption intensities were measured. The obtained results proved that ethanolic extract showed absorption peaks attributed to: phenolic compounds (free phenolic acids and phenolic acids derivatives) registrated between 220-280 nm, unsymmetrical chemical structure compounds (caffeic acid, chlorogenic acid, ferulic acid) with maximum absorption peak and absorption "shoulder" that may be due to substitution of hydroxyl or methoxy group, flavonoid compounds (in free form or glycosides) between 330-360 nm, due to the double bond in position 2,3 and carbonyl group in position 4 flavonols. UV spectra showed two major peaks of absorption (quercetin glycoside, rutin, etc.). The results obtained by UV-VIS spectroscopy has revealed the presence of phenolic derivatives such as cicoric acid (240 nm), caftaric acid (329 nm), caffeic acid (240 nm), rutoside (205 nm), quercetin (255 nm), luteolin (235 nm) in all three species of Echinacea. The echinacoside is absent. This profile mentioned above and the absence of phenolic compound echinacoside leads to the conclusion that species harvested as Echinacea angustifolia and Echinacea pallida are Echinacea purpurea also; It can be said that preliminary fingerprinting of Echinacea species through correspondence with the phenolic derivatives profile can be achieved by UV-VIS spectroscopic investigation, which is an adequate technique for preliminary identification and authentication of Echinacea in medicinal herbs.Keywords: Echinacea species, Fingerprinting, Phenolic compounds, UV-VIS spectroscopy
Procedia PDF Downloads 2611704 Chemical Composition, Antioxidant and Antibacterial Activities of Essential Oil from the Leaves of Thymus vulgaris L.
Authors: Tsige Reda
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Essential oil of Thymus vulgaris was extracted by means of hydro-distillation. This study was done to investigate the chemical composition, antibacterial and antioxidant activities. The chemical composition of the essential oils was determined using gas chromatography coupled to mass spectroscopy (GC-MS). Using disc diffusion assay the antibacterial activity was assessed on one Gram-positive bacteria and one Gram-negative bacteria. The percentage oil yield of the essential oil was found to be 0.97 ± 0.08% (w/w) with yellow color. The physicochemical constants of the oil were also noted. The phytochemical screening of the plant extract revealed the presence of tannins, saponins, phenol, flavonoids, terpenoids, steroids and alkaloids. A total of 18 chemical constituents were identified by Gas Chromatography-Mass Spectroscopy analysis representing 100% of the total essential oil of Thymus vulgaris, with thymol (31.977%), o-cymene (29.992%), and carvacrol (14.541%). Previous studies have revealed that the thymol, o-cymen and carvacrol components of Thymus vulgaris are responsible for their biological activities. Thymus vulgaris have been used traditionally to treat a wide variety of infections. Based on the extensive use and lack of scientific evidence, a study was embarked upon to determine its bioactivity. The essential oil of Thymus vulgaris leaves exhibited higher activity towards the Gram-positive bacteria (Staphylococcus aurous) than the Gram-negative bacteria (Escherichia coli) and also has good antioxidant activity, and can be used medicinal and therapeutic applications. This activity may be due to the high amount of thymol, o-cymen and carvacrol.Keywords: hydro-distillation, Thymus vulgaris, essential oil composition, phytochemical screening, physicochemical constants, antioxidant activity, antibacterial activity
Procedia PDF Downloads 4371703 Pt Decorated Functionalized Acetylene Black as Efficient Cathode Material for Li Air Battery and Fuel Cell Applications
Authors: Rajashekar Badam, Vedarajan Raman, Noriyoshi Matsumi
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Efficiency of energy converting and storage systems like fuel cells and Li-Air battery principally depended on oxygen reduction reaction (ORR) which occurs at cathode. As the kinetics of the ORR is very slow, it becomes the rate determining step. Exploring carbon substrates for enhancing the dispersion and activity of the metal catalyst and commercially viable simple preparation method is a very crucial area of research in the field of energy materials. Hence, many researchers made large number of carbon-based ORR materials today. But, there are hardly few studies on the effect of interaction between Pt-carbon and carbon-electrolyte on activity. In this work, we have prepared functionalized carbon-based Pt catalyst (Pt-FAB) with enhanced interfacial properties that lead to efficient ORR catalysis. The present work deals with a single-pot method to exfoliate and functionalized acetylene black with enhanced interaction with Pt as well as electrolyte. Acetylene black was functionalized and exfoliated using a facile single pot acid treatment method. The resulted FAB was further decorated with Pt-nano particles (Pt-np). The TEM images of Pt-FAB with uniformly decorated Pt-np of ~3 nm. Further, XPS studies of Pt 4f peak revealed that Pt0 peak was shifted by 0.4 eV in Pt-FAB compared to binding energy of typical Pt⁰ found in Pt/C. The shift can be ascribed to the modulation of electronic state and strong electronic interaction of Pt with carbon. Modulated electronic structure of Pt and strong electronic interaction of Pt with FAB enhances the catalytic activity and durability respectively. To understand the electrode electrolyte interface, electrochemical impedance spectroscopy was carried out. These measurements revealed that the charge transfer resistance of electrode to electrolyte for Pt-FAB is 10 times smaller than that of conventional Pt/C. The interaction with electrolyte helps reduce the interface boundaries, which in turn affects the overall catalytic performance of the electrode. Cyclic voltammetric measurements in 0.1M HClO₄ aq. at a potential scan rate of 50 mVs-1 was employed to evaluate electrochemical surface area (ECSA) of Pt. ECSA of Pt-FAB was found to be as high as 67.2 m²g⁻¹. The three-electrode system showed very high ORR catalytic activity. Mass activity at 0.9 V vs. RHE showed 460 A/g which is much higher than the DOE target values for the year 2020. Further, it showed enhanced performance by showing 723 mW/cm² of highest power density and 1006 mA/cm² of current density at 0.6 V in fuel cell single cell type configuration and 1030 mAhg⁻¹ of rechargeable capacity in Li air battery application. The higher catalytic activity can be ascribed to the improved interaction of FAB with Pt and electrolyte. The aforementioned results evince that Pt-FAB will be a promising cathode material for efficient ORR with significant cyclability for its application in fuel cells and Li-Air batteries. In conclusion, a disordered material was prepared from AB and was systematically characterized. The extremely high ORR activity and ease of preparation make it competent for replacing commercially available ORR materials.Keywords: functionalized acetylene black, oxygen reduction reaction, fuel cells, Functionalized battery
Procedia PDF Downloads 1081702 Effect of Li-excess on Electrochemical Performance of Ni-rich LiNi₀.₉Co₀.₀₉Mn₀.₀₉O₂ Cathode Materials for Li-ion Batteries
Authors: Eyob Belew Abebe
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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 1751701 Green Synthesis of Silver and Silver-Gold Alloy Nanoparticle Using Cyanobacteria as Bioreagent
Authors: Piya Roychoudhury, Ruma Pal
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Cyanobacteria, commonly known as blue green algae were found to be an effective bioreagent for nanoparticle synthesis. Nowadays silver nanoparticles (AgNPs) are very popular due to their antimicrobial and anti-proliferative activity. To exploit these characters in different biotechnological fields, it is very essential to synthesize more stable, non-toxic nano-silver. For this reason silver-gold alloy (Ag-AuNPs) nanoparticles are of great interest as they are more stable, harder and more effective than single metal nanoparticles. In the present communication we described a simple technique for rapid synthesis of biocompatible AgNP and Ag-AuNP employing cyanobacteria, Leptolyngbya and Lyngbya respectively. For synthesis of AgNP the biomass of Leptolyngbya valderiana (200 mg Fresh weight) was exposed to 9 mM AgNO3 solution (pH 4). For synthesis of Ag-AuNP Lyngbya majuscula (200 mg Fresh weight) was exposed to equimolar solution of hydrogen tetra-auro chlorate and silver nitrate (1mM, pH 4). After 72 hrs of exposure thallus of Leptolyngyba turned brown in color and filaments of Lyngbya turned pink in color that indicated synthesis of nanoparticles. The produced particles were extracted from the cyanobacterial biomass using nano-capping agent, sodium citrate. Firstly, extracted brown and pink suspensions were taken for Energy Dispersive X-ray (EDAX) analysis to confirm the presence of silver in brown suspension and presence of both gold and silver in pink suspension. Extracted nanoparticles showed a distinct single plasmon band (AgNP at 411 nm; Ag-Au NP at 481 nm) in Uv-vis spectroscopy. It was revealed from Transmission electron microscopy (TEM) that all the synthesized particles were spherical in nature with a size range of ~2-25 nm. In X-ray powder diffraction (XRD) analysis four intense peaks appeared at 38.2°, 44.5°, 64.8°and 77.8° which confirmed the crystallographic nature of synthesized particles. Presence of different functional groups viz. N-H, C=C, C–O, C=O on the surface of nanoparticles were recorded by Fourier transform infrared spectroscopy (FTIR). Scanning Electron microscopy (SEM) images showed the surface topography of metal treated filaments of cyanobacteria. The stability of the particles was observed by Zeta potential study. Antibiotic property of synthesized particles was tested by Agar well diffusion method against gram negative bacteria Pseudomonas aeruginosa. Overall, this green-technique requires low energy, less manufacturing cost and produces rapidly eco-friendly metal nanoparticles.Keywords: cyanobacteria, silver nanoparticles, silver-gold alloy nanoparticles, spectroscopy
Procedia PDF Downloads 3231700 Ferrites of the MeFe2O4 System (Me – Zn, Cu, Cd) and Their Two Faces
Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov
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The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite
Procedia PDF Downloads 4361699 Removal of Lead Ions from Aqueous Medium Using Devised Column Filters Packed with Chitosan from Trash Crab Shells: A Characterization Study
Authors: Charles Klein O. Gorit, Mark Tristan J. Quimque Jr., M. Cecilia V. Almeda, Concepcion M. Salvana
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Chitosan is a promising biopolymer commonly found in crustacean shells that has plausible effects in water purification and wastewater treatment. It is a primary derivative of chitin and considered second of the most abundant biopolymer prior to cellulose. Morphological analysis had been done using Scanning Electron Microscopy with Energy Dispersive Microscopy (SEM/EDS), and due to its porous nature, it showcases a certain degree of porosity, hence, larger adsorption site of heavy metal. The Energy Dispersive Spectroscopy of the chitosan and ‘lead-bound’ chitosan, shows a relative increase of percent abundance of lead cation from 1.44% to 2.08% hence, adsorption occurs. Chitosan, as a nitrogenous polysaccharide, subjected to Fourier transform infrared spectroscopy (FTIR) analysis shows amide bands ranging from 1635.36 cm⁻¹ for amide 1 band and 1558.40 cm-1 for amide 2 band with NH stretching. For ‘lead-bound’ chitosan, the FT-IR analysis shows a change in peaks upon adsorption of Pb(II) cation. The spectrum shows broadening of OH and NH stretching band. Such observation can be attributed to the probability that the attachment of Pb(II) ions is in these functional groups. A column filter was devised with lead-bound chitosan to determine the zero point charge (pHzpc) of the biopolymer. The results show that at pH 8.34, below than the zpc level of literatures cited for lead which ranges from pH 4 to 7, favors the adsorption site of chitosan and its capability to adsorb traces amount of aqueous lead.Keywords: chitosan, biopolymer, FT-IR, SEM, zero-point charge, heavy metal, lead ions
Procedia PDF Downloads 1511698 Electrochemical Modification of Boron Doped Carbon Nanowall Electrodes for Biosensing Purposes
Authors: M. Kowalski, M. Brodowski, K. Dziabowska, E. Czaczyk, W. Bialobrzeska, N. Malinowska, S. Zoledowska, R. Bogdanowicz, D. Nidzworski
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Boron-doped-carbon nanowall (BCNW) electrodes are recently in much interest among scientists. BCNWs are good candidates for biosensor purposes as they possess interesting electrochemical characteristics like a wide potential range and the low difference between redox peaks. Moreover, from technical parameters, they are mechanically resistant and very tough. The production process of the microwave plasma-enhanced chemical vapor deposition (MPECVD) allows boron to build into the structure of the diamond being formed. The effect is the formation of flat, long structures with sharp ends. The potential of these electrodes was checked in the biosensing field. The procedure of simple carbon electrodes modification by antibodies was adopted to BCNW for specific antigen recognition. Surface protein D deriving from H. influenzae pathogenic bacteria was chosen as a target analyte. The electrode was first modified with the aminobenzoic acid diazonium salt by electrografting (electrochemical reduction), next anti-protein D antibodies were linked via 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride/N-hydroxysuccinimide (EDC/NHS) chemistry, and free sites were blocked by BSA. Cyclic voltammetry measurements confirmed the proper electrode modification. Electrochemical impedance spectroscopy records indicated protein detection. The sensor was proven to detect protein D in femtograms. This work was supported by the National Centre for Research and Development (NCBR) TECHMATSTRATEG 1/347324/12/NCBR/ 2017.Keywords: anti-protein D antibodies, boron-doped carbon nanowall, impedance spectroscopy, Haemophilus influenzae.
Procedia PDF Downloads 1731697 Physio-Thermal and Geochemical Behavior and Alteration of the Au Pathfinder Gangue Hydrothermal Quartz at the Kubi Gold Ore Deposits
Authors: Gabriel K. Nzulu, Lina Rostorm, Hans Högberg, Jun Liu, per Eklund, Lars Hultman, Martin Magnuson
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Altered and gangue quartz in hydrothermal veins from the Kubi Gold deposit in Dunkwa on Offin in the central region of Ghana are investigated for possible Au associated pathfinder minerals and to provide understanding and increase the knowledge of the mineral hosting and alteration processes in quartz. X-ray diffraction, air annealing furnace, differential scanning calorimetry, energy dispersive X-ray spectroscopy, and transmission electron microscopy have been applied on different quartz types outcropping from surface and bed rocks at the Kubi Gold Mining to reveal the material properties at different temperatures. From the diffraction results of the fresh and annealed quartz samples, we find that the samples contain pathfinder and the impurity minerals FeS₂, biotite, TiO₂, and magnetite. These minerals, under oxidation process between 574-1400 °C temperatures experienced hematite alterations and a transformation from α-quartz to β-quartz and further to cristobalite as observed from the calorimetry scans for hydrothermally exposed materials. The energy dispersive spectroscopy revealed elemental species of Fe, S, Mg, K, Al, Ti, Na, Si, O, and Ca contained in the samples and these are attributed to the impurity phase minerals observed in the diffraction. The findings also suggest that during the hydrothermal flow regime, impurity minerals and metals can be trapped by voids and faults. Under favorable temperature conditions the trapped minerals can be altered to change color at different depositional stages by oxidation and reduction processes leading to hematite alteration which is a useful pathfinder in mineral exploration.Keywords: quartz, hydrothermal, minerals, hematite, x-ray diffraction, crystal-structure, defects
Procedia PDF Downloads 971696 Collagen Silver Lipid Nanoparticles as Matrix and Fillers for Cosmeceuticals: An In-Vitro and In-Vivo Study
Authors: Kumari Kajal, Muthu Kumar Sampath, Hare Ram Singh
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In this context, the formulation and characterization of collagen silver lipid nanoparticles (CSLNs) were studied for their capacity to serve as fillers/matrix materials used in cosmeceutical applications. The CSLNs were prepared following a series of studies, such as X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) coupled with energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy FT-IR; thermogravimetric analysis (TGA); and differential scanning calorimetry (DSC). The studies confirmed the structural integrity of nanoparticles, their cargo and thermal stability. The biological functionality of CSLNs was studied by carrying out in vitro & in vivo studies. The antibacterial effect, hemocompatibility and anti-inflammatory characteristics of these fibers were systematically investigated. The toxicological assays included oral toxicity in mice and aquatic life tests with the fish Danio rerio model. The morphology of the nanoparticles was confirmed using high-resolution transmission electron microscopy (HR-TEM). The report found that CSLNs had strong antimicrobial effects, unmatched hemocompatibility, and low or absent inflammatory reactions, which makes them perfect candidates for cosmeceutical applications. The toxicological evaluations evinced a good safety record without any significant adverse effects in both murine and Danio rerio models. This research reveals the efficient way of CSLNs to the efficacy and safety of dermaceuticals.Keywords: collagen silver lipid nanoparticles (CSLNs), cosmeceuticals, antimicrobial activity, hemocompatibility, in vitro assessment, in vivo assessment.
Procedia PDF Downloads 171695 Application of Electrochemical Impedance Spectroscopy to Monitor the Steel/Soil Interface During Cathodic Protection of Steel in Simulated Soil Solution
Authors: Mandlenkosi George Robert Mahlobo, Tumelo Seadira, Major Melusi Mabuza, Peter Apata Olubambi
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Cathodic protection (CP) has been widely considered a suitable technique for mitigating corrosion of buried metal structures. Plenty of efforts have been made in developing techniques, in particular non-destructive techniques, for monitoring and quantifying the effectiveness of CP to ensure the sustainability and performance of buried steel structures. The aim of this study was to investigate the evolution of the electrochemical processes at the steel/soil interface during the application of CP on steel in simulated soil. Carbon steel was subjected to electrochemical tests with NS4 solution used as simulated soil conditions for 4 days before applying CP for a further 11 days. A previously modified non-destructive voltammetry technique was applied before and after the application of CP to measure the corrosion rate. Electrochemical impedance spectroscopy (EIS), in combination with mathematical modeling through equivalent electric circuits, was applied to determine the electrochemical behavior at the steel/soil interface. The measured corrosion rate was found to have decreased from 410 µm/yr to 8 µm/yr between days 5 and 14 because of the applied CP. Equivalent electrical circuits were successfully constructed and used to adequately model the EIS results. The modeling of the obtained EIS results revealed the formation of corrosion products via a mixed activation-diffusion mechanism during the first 4 days, while the activation mechanism prevailed in the presence of CP, resulting in a protective film. The x-ray diffraction analysis confirmed the presence of corrosion products and the predominant protective film corresponding to the calcareous deposit.Keywords: carbon steel, cathodic protection, NS4 solution, voltammetry, EIS
Procedia PDF Downloads 641694 Surface Induced Alteration of Nanosized Amorphous Alumina
Authors: A. Katsman, L. Bloch, Y. Etinger, Y. Kauffmann, B. Pokroy
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Various nanosized amorphous alumina thin films in the range of (2.4 - 63.1) nm were deposited onto amorphous carbon and amorphous Si3N4 membrane grids. Transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), X-ray photoelectron spectroscopy (XPS) and differential scanning calorimetry (DSC) techniques were used to probe the size effect on the short range order and the amorphous to crystalline phase transition temperature. It was found that the short-range order changes as a function of size: the fraction of tetrahedral Al sites is greater in thinner amorphous films. This result correlates with the change of amorphous alumina density with the film thickness demonstrated by the reflectivity experiments: the thinner amorphous films have the less density. These effects are discussed in terms of surface reconstruction of the amorphous alumina films. The average atomic binding energy in the thin film layer decreases with decease of the thickness, while the average O-Al interatomic distance increases. The reconstruction of amorphous alumina is induced by the surface reconstruction, and the short range order changes being dependent on the density. Decrease of the surface energy during reconstruction is the driving force of the alumina reconstruction (density change) followed by relaxation process (short range order change). The amorphous to crystalline phase transition temperature measured by DSC rises with the decrease in thickness from 997.6°C for 13.9 nm to 1020.4 °C for 2.7 nm thick. This effect was attributed to the different film densities: formation of nanovoids preceding and accompanying crystallization process influences the crystallization rate, and by these means, the temperature of crystallization peak.Keywords: amorphous alumina, density, short range order, size effect
Procedia PDF Downloads 4661693 Clinical Validation of C-PDR Methodology for Accurate Non-Invasive Detection of Helicobacter pylori Infection
Authors: Suman Som, Abhijit Maity, Sunil B. Daschakraborty, Sujit Chaudhuri, Manik Pradhan
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Background: Helicobacter pylori is a common and important human pathogen and the primary cause of peptic ulcer disease and gastric cancer. Currently H. pylori infection is detected by both invasive and non-invasive way but the diagnostic accuracy is not up to the mark. Aim: To set up an optimal diagnostic cut-off value of 13C-Urea Breath Test to detect H. pylori infection and evaluate a novel c-PDR methodology to overcome of inconclusive grey zone. Materials and Methods: All 83 subjects first underwent upper-gastrointestinal endoscopy followed by rapid urease test and histopathology and depending on these results; we classified 49 subjects as H. pylori positive and 34 negative. After an overnight, fast patients are taken 4 gm of citric acid in 200 ml water solution and 10 minute after ingestion of the test meal, a baseline exhaled breath sample was collected. Thereafter an oral dose of 75 mg 13C-Urea dissolved in 50 ml water was given and breath samples were collected upto 90 minute for 15 minute intervals and analysed by laser based high precisional cavity enhanced spectroscopy. Results: We studied the excretion kinetics of 13C isotope enrichment (expressed as δDOB13C ‰) of exhaled breath samples and found maximum enrichment around 30 minute of H. pylori positive patients, it is due to the acid mediated stimulated urease enzyme activity and maximum acidification happened within 30 minute but no such significant isotopic enrichment observed for H. pylori negative individuals. Using Receiver Operating Characteristic (ROC) curve an optimal diagnostic cut-off value, δDOB13C ‰ = 3.14 was determined at 30 minute exhibiting 89.16% accuracy. Now to overcome grey zone problem we explore percentage dose of 13C recovered per hour, i.e. 13C-PDR (%/hr) and cumulative percentage dose of 13C recovered, i.e. c-PDR (%) in exhaled breath samples for the present 13C-UBT. We further explored the diagnostic accuracy of 13C-UBT by constructing ROC curve using c-PDR (%) values and an optimal cut-off value was estimated to be c-PDR = 1.47 (%) at 60 minute, exhibiting 100 % diagnostic sensitivity , 100 % specificity and 100 % accuracy of 13C-UBT for detection of H. pylori infection. We also elucidate the gastric emptying process of present 13C-UBT for H. pylori positive patients. The maximal emptying rate found at 36 minute and half empting time of present 13C-UBT was found at 45 minute. Conclusions: The present study exhibiting the importance of c-PDR methodology to overcome of grey zone problem in 13C-UBT for accurate determination of infection without any risk of diagnostic errors and making it sufficiently robust and novel method for an accurate and fast non-invasive diagnosis of H. pylori infection for large scale screening purposes.Keywords: 13C-Urea breath test, c-PDR methodology, grey zone, Helicobacter pylori
Procedia PDF Downloads 3011692 Development of Alpha Spectroscopy Method with Solid State Nuclear Track Detector Using Aluminium Thin Films
Authors: Nidal Dwaikat
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This work presents the development of alpha spectroscopy method with Solid-state nuclear track detectors using aluminum thin films. The resolution of this method is high, and it is able to discriminate between alpha particles at different incident energy. It can measure the exact number of alpha particles at specific energy without needing a calibration of alpha track diameter versus alpha energy. This method was tested by using Cf-252 alpha standard source at energies 5.11 Mev, 3.86 MeV and 2.7 MeV, which produced by the variation of detector -standard source distance. On front side, two detectors were covered with two Aluminum thin films and the third detector was kept uncovered. The thickness of Aluminum thin films was selected carefully (using SRIM 2013) such that one of the films will block the lower two alpha particles (3.86 MeV and 2.7 MeV) and the alpha particles at higher energy (5.11 Mev) can penetrate the film and reach the detector’s surface. The second thin film will block alpha particles at lower energy of 2.7 MeV and allow alpha particles at higher two energies (5.11 Mev and 3.86 MeV) to penetrate and produce tracks. For uncovered detector, alpha particles at three different energies can produce tracks on it. For quality assurance and accuracy, the detectors were mounted on thick enough copper substrates to block exposure from the backside. The tracks on the first detector are due to alpha particles at energy of 5.11 MeV. The difference between the tracks number on the first detector and the tracks number on the second detector is due to alpha particles at energy of 3.8 MeV. Finally, by subtracting the tracks number on the second detector from the tracks number on the third detector (uncovered), we can find the tracks number due to alpha particles at energy 2.7 MeV. After knowing the efficiency calibration factor, we can exactly calculate the activity of standard source.Keywords: aluminium thin film, alpha particles, copper substrate, CR-39 detector
Procedia PDF Downloads 3651691 In Vivo Assessment of Biogenically Synthesized Silver Nanoparticles
Authors: Muhammad Shahzad Tufail, Iram Liaqat
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Silver nanoparticles (AgNPs) have wider biomedical applications due to their intensive antimicrobial activities. However, toxicity and side effects of nanomaterials like AgNPs is a subject of great controversy towards the further studies in this direction. In this study, biogenically synthesized AgNPs, previously characterized via ultraviolet (UV) visible spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR), were subjected to toxicity evaluation using mice model. Albino male mice (BALB/c) were administered with 50 mgkg-1, 100 mgkg-1 and 150 mgkg-1 of AgNPs, respectively, except for control for 30 days. Log-probit regression analysis was used to measure the dosage response to determine the median lethal dose (LD50). Exposure to AgNPs caused significant changes in the levels of serum AST (P ˂ 0.05) at the 100mgkg-1 and 150mgkg-1 of AgNPs exposure, while ALT and serum creatinine (P ˃ 0.05) levels remained normal. Histopathology of male albino mice liver and kidney was studied after 30 days experimental period. Results revealed that mice exposed to heavy dose (150 mgkg-1) of AgNPs showed cell distortion, necrosis and detachment of hepatocytes in the liver. Regarding kidney, at lower concentration, normal renal structure with normal glomeruli was observed. However, at higher concentration (150 mgkg-1), kidneys showed smooth surface and dark red colour with proliferation of podocytes. It can be concluded from present study that biologically synthesized AgNPs are small to be eliminated easily by kidney and therefore the liver and kidney did not show toxicity at low concentrations.Keywords: silver nanoparticles, pseudomonas aeruginosa, male albino mice, toxicity assessment
Procedia PDF Downloads 791690 Tailoring Structural, Thermal and Luminescent Properties of Solid-State MIL-53(Al) MOF via Fe³⁺ Cation Exchange
Authors: T. Ul Rehman, S. Agnello, F. M. Gelardi, M. M. Calvino, G. Lazzara, G. Buscarino, M. Cannas
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Metal-Organic Frameworks (MOFs) have emerged as promising candidates for detecting metal ions owing to their large surface area, customizable porosity, and diverse functionalities. In recent years, there has been a surge in research focused on MOFs with luminescent properties. These frameworks are constructed through coordinated bonding between metal ions and multi-dentate ligands, resulting in inherent fluorescent structures. Their luminescent behavior is influenced by factors like structural composition, surface morphology, pore volume, and interactions with target analytes, particularly metal ions. MOFs exhibit various sensing mechanisms, including photo-induced electron transfer (PET) and charge transfer processes such as ligand-to-metal (LMCT) and metal-to-ligand (MLCT) transitions. Among these, MIL-53(Al) stands out due to its flexibility, stability, and specific affinity towards certain metal ions, making it a promising platform for selective metal ion sensing. This study investigates the structural, thermal, and luminescent properties of MIL-53(Al) metal-organic framework (MOF) upon Fe3+ cation exchange. Two separate sets of samples were prepared to activate the MOF powder at different temperatures. The first set of samples, referred to as MIL-53(Al), activated (120°C), was prepared by activating the raw powder in a glass tube at 120°C for 12 hours and then sealing it. The second set of samples, referred to as MIL-53(Al), activated (300°C), was prepared by activating the MIL-53(Al) powder in a glass tube at 300°C for 70 hours. Additionally, 25 mg of MIL-53(Al) powder was dispersed in 5 mL of Fe3+ solution at various concentrations (0.1-100 mM) for the cation exchange experiment. The suspension was centrifuged for five minutes at 10,000 rpm to extract MIL-53(Al) powder. After three rounds of washing with ultrapure water, MIL-53(Al) powder was heated at 120°C for 12 hours. For PXRD and TGA analyses, a sample of the obtained MIL-53(Al) was used. We also activated the cation-exchanged samples for time-resolved photoluminescence (TRPL) measurements at two distinct temperatures (120 and 300°C) for comparative analysis. Powder X-ray diffraction patterns reveal amorphization in samples with higher Fe3+ concentrations, attributed to alterations in coordination environments and ion exchange dynamics. Thermal decomposition analysis shows reduced weight loss in Fe3+-exchanged MOFs, indicating enhanced stability due to stronger metal-ligand bonds and altered decomposition pathways. Raman spectroscopy demonstrates intensity decrease, shape disruption, and frequency shifts, indicative of structural perturbations induced by cation exchange. Photoluminescence spectra exhibit ligand-based emission (π-π* or n-π*) and ligand-to-metal charge transfer (LMCT), influenced by activation temperature and Fe3+ incorporation. Quenching of luminescence intensity and shorter lifetimes upon Fe3+ exchange result from structural distortions and Fe3+ binding to organic linkers. In a nutshell, this research underscores the complex interplay between composition, structure, and properties in MOFs, offering insights into their potential for diverse applications in catalysis, gas storage, and luminescent devices.Keywords: Fe³⁺ cation exchange, luminescent metal-organic frameworks (LMOFs), MIL-53(Al), solid-state analysis
Procedia PDF Downloads 661689 Active Thermography Technique for High-Entropy Alloy Characterization Deposited with Cold Spray Technique
Authors: Nazanin Sheibanian, Raffaella Sesana, Sedat Ozbilen
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In recent years, high-entropy alloys (HEAs) have attracted considerable attention due to their unique properties and potential applications. In this study, novel HEA coatings were prepared on Mg substrates using mechanically alloyed HEA powder feedstocks based on Al_(0.1-0.5)CoCrCuFeNi and MnCoCrCuFeNi multi-material systems. The coatings were deposited by the Cold Spray (CS) process using three different temperatures of the process gas (N2) (650°C, 750°C, and 850°C) to examine the effect of gas temperature on coating properties. In this study, Infrared Thermography (non-destructive) was examined as a possible quality control technique for HEA coatings applied to magnesium substrates. Active Thermography was employed to characterize coating properties using the thermal response of the coating. Various HEA chemical compositions and deposition temperatures have been investigated. As a part of this study, a comprehensive macro and microstructural analysis of Cold Spray (CS) HEA coatings has been conducted using macrophotography, optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM+EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microhardness tests, roughness measurements, and porosity assessments. These analyses provided insight into phase identification, microstructure characterization, deposition, particle deformation behavior, bonding mechanisms, and identifying a possible relationship between physical properties and thermal responses. Based on the figures and tables, it is evident that the Maximum Relative Radiance (∆RMax) of each sample differs depending on both the chemical composition of HEA and the temperature at which Cold Spray is applied.Keywords: active thermography, coating, cold spray, high- entropy alloy, material characterization
Procedia PDF Downloads 721688 Geomatic Techniques to Filter Vegetation from Point Clouds
Authors: M. Amparo Núñez-Andrés, Felipe Buill, Albert Prades
Abstract:
More and more frequently, geomatics techniques such as terrestrial laser scanning or digital photogrammetry, either terrestrial or from drones, are being used to obtain digital terrain models (DTM) used for the monitoring of geological phenomena that cause natural disasters, such as landslides, rockfalls, debris-flow. One of the main multitemporal analyses developed from these models is the quantification of volume changes in the slopes and hillsides, either caused by erosion, fall, or land movement in the source area or sedimentation in the deposition zone. To carry out this task, it is necessary to filter the point clouds of all those elements that do not belong to the slopes. Among these elements, vegetation stands out as it is the one we find with the greatest presence and its constant change, both seasonal and daily, as it is affected by factors such as wind. One of the best-known indexes to detect vegetation on the image is the NVDI (Normalized Difference Vegetation Index), which is obtained from the combination of the infrared and red channels. Therefore it is necessary to have a multispectral camera. These cameras are generally of lower resolution than conventional RGB cameras, while their cost is much higher. Therefore we have to look for alternative indices based on RGB. In this communication, we present the results obtained in Georisk project (PID2019‐103974RB‐I00/MCIN/AEI/10.13039/501100011033) by using the GLI (Green Leaf Index) and ExG (Excessive Greenness), as well as the change to the Hue-Saturation-Value (HSV) color space being the H coordinate the one that gives us the most information for vegetation filtering. These filters are applied both to the images, creating binary masks to be used when applying the SfM algorithms, and to the point cloud obtained directly by the photogrammetric process without any previous filter or the one obtained by TLS (Terrestrial Laser Scanning). In this last case, we have also tried to work with a Riegl VZ400i sensor that allows the reception, as in the aerial LiDAR, of several returns of the signal. Information to be used for the classification on the point cloud. After applying all the techniques in different locations, the results show that the color-based filters allow correct filtering in those areas where the presence of shadows is not excessive and there is a contrast between the color of the slope lithology and the vegetation. As we have advanced in the case of using the HSV color space, it is the H coordinate that responds best for this filtering. Finally, the use of the various returns of the TLS signal allows filtering with some limitations.Keywords: RGB index, TLS, photogrammetry, multispectral camera, point cloud
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