Search results for: high performance thin layer chromatography

Authors: Philipp Stehle, Dragoljub Vrankovic, Montaha Anjass

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Due to its high availability and extremely high specific capacity, silicon (Si) is the most promising anode material for next generation lithium-ion batteries (LIBs). However, Si anodes are suffering from high volume changes during cycling causing unstable solid-electrolyte interface (SEI). One approach for mitigation of these effects is to embed Si particles into a carbon matrix to create silicon/carbon composites (Si/C). These typically show more stable electrochemical performance than bare silicon materials. Nevertheless, the same failure mechanisms mentioned earlier appear in a less pronounced form. In this work, we further improved the cycling performance of two commercially available Si/C materials by coating thin metal oxide films of different thicknesses on the powders via Atomic Layer Deposition (ALD). The coated powders were analyzed via ICP-OES and AFM measurements. Si/C-graphite anodes with automotive-relevant loadings (~3.5 mAh/cm2) were processed out of the materials and tested in half coin cells (HCCs) and full pouch cells (FPCs). During long-term cycling in FPCs, a significant improvement was observed for some of the ALD-coated materials. After 500 cycles, the capacity retention was already up to 10% higher compared to the pristine materials. Cycling of the FPCs continued until they reached a state of health (SOH) of 80%. By this point, up to the triple number of cycles were achieved by ALD-coated compared to pristine anodes. Post-mortem analysis via various methods was carried out to evaluate the differences in SEI formation and thicknesses.

Keywords: silicon anodes, li-ion batteries, atomic layer deposition, silicon-carbon composites, surface coatings

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Authors: M. L. Ibrahim, A. Abdulhamid

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A surface active molecule synthesized by a rhizobacterial strain Bacillus lentus isolated from Cajanus cajan was investigated. The bioemulsifier was extracted, purified and partially characterized using standard methods. Surface properties of the bioemulsifier were determined by studying the emulsification index, solubility test and stability studies. Partial purification of the bioemulsifier was carried out using FT-IR analysis, Silica-gel column chromatography and thin layer chromatography. GC-MS analysis was carried out to detect the composition and mass of the lipids and esters. The isolate showed an emulsifying activity of 57% and surface activity of 36mm. The stability studies revealed that the bioemulsifier had better stability at temperature of 70oC, 8% pH and 8% NaCl concentration. FT-IR indicated the bioemulsifier to contain peptide and aliphatic chain, TLC revealed the compound to be ninhydrin positive and Column chromatography showed the presence of three amino acids namely; glutamine, valine and cysteine. GC-MS indicated the lipid moiety to contain aliphatic chain ranging from C9-C16 and two major peaks of 1,2-benzenedicarboxylic acid diethyl octyl ester. Therefore, surface active agent from Bacillus lentus can be used effectively in a wide range of applications such as in MEOR and in the biosynthesis of plasticizers for industrial uses.

Keywords: Bacillus lentus, bioemulsifiers, phthalic acid ester, Rhizosphere

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Authors: Reza Pashaei, Reda Dzingelevičienė

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An efficient, reliable, and sensitive multiclass analytical method has been expanded to simultaneously determine 15 human pharmaceutical residues in fish and shrimp tissue samples by ultra-high-performance liquid chromatography-tandem mass spectrometry. The investigated compounds comprise ten classes, namely analgesic, antibacterial, anticonvulsant, cardiovascular, fluoroquinolones, macrolides, nonsteroidal anti-inflammatory, penicillins, stimulant, and sulfonamide. A simple liquid extraction procedure based on 0.1% formic acid in methanol was developed. Chromatographic conditions were optimized, and mobile phase namely 0.1 % ammonium acetate (A), and acetonitrile (B): 0 – 2 min, 15% B; 2 – 5 min, linear to 95% B; 5 – 10 min, 95% B; and 10 – 12 min was obtained. Limits of detection and quantification ranged from 0.017 to 1.371 μg/kg and 0.051 to 4.113 μg/kg, respectively. Finally, amoxicillin, azithromycin, caffeine, carbamazepine, ciprofloxacin, clarithromycin, diclofenac, erythromycin, furosemide, ibuprofen, ketoprofen, naproxen, sulfamethoxazole, tetracycline, and triclosan were quantifiable in fish and shrimp samples.

Keywords: fish, liquid chromatography, mass spectrometry, pharmaceuticals, shrimp, solid-phase extraction

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Authors: Radia Kamel

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Considerable progress has been made in the development of bulk-heterojunction organic solar cells (OSCs) based on a blend of p-type and n-type organic semiconductors. To optimize the interfacial properties between the active layer and the electrode, a cathode buffer layer (CBL) is introduced. This layer can reduce the leakage current, increasing the open-circuit voltage and the fill factor while improving the OSC stability. In this work, the performance of PM6:Y6 OSC with 1-Chloronaphthalene as an additive is examined. To accomplish this, three CBLs PNDIT-F3N-Br, ZrAcac, and PDINO, are compared using the conventional configuration. The device with PNDIT-F3N-Br as CBL exhibits the highest power conversion efficiency of 16.04%. The results demonstrate that modifying the cathode buffer layer is crucial for achieving high-performance OSCs.

Keywords: bulk heterojunction, cathode buffer layer, efficiency, organic solar cells

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Authors: Damian A. Mooney, Michael T. P. Mc Cann, J. M. Don MacElroy, Olli Antson, Denis P. Dowling

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Atmospheric pressure plasma liquid deposition (APPLD) is a novel technology used for the deposition of thin films via the injection of a reactive liquid precursor into a high-energy discharge plasma at ambient pressure. In this work, APPLD, utilising a TEOS precursor, was employed to produce asymmetric membranes consisting of a thin (100 nm) layer of deposited silica on a microporous silica support in order to assess their suitability for high temperature gas separation applications. He and N₂ gas permeability measurements were made for each of the fabricated membranes and a maximum ideal He/N₂ selectivity of 66 was observed at room temperature. He, N₂ and CO2 gas permeances were also measured at the elevated temperature of 673K and ideal He/N₂ and CO₂/N₂ selectivities of 300 and 7.4, respectively, were observed. The results suggest that this plasma-based deposition technique can be a viable method for the manufacture of membranes for the efficient separation of high temperature, post-combustion gases, including that of CO₂/N₂ where the constituent gases differ in size by fractions of an Ångstrom.

Keywords: asymmetric membrane, CO₂ separation, high temperature, plasma deposition, thin films

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Authors: Pouyan Motamedi, Ken Bosnick, Ken Cadien, James Hogan

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Growth of conformal ultrathin metal films has attracted a considerable amount of attention recently. Plasma-enhanced atomic layer deposition (PEALD) is a method capable of growing conformal thin films at low temperatures, with an exemplary control over thickness. The authors have recently reported on growth of metastable epitaxial nickel thin films via PEALD, along with a comprehensive characterization of the films and a study on the relationship between the growth parameters and the film characteristics. The goal of the current study is to use the mentioned films as a case study to investigate the temperature-activated phase transformation and agglomeration in ultrathin metallic films. For this purpose, metastable hexagonal nickel thin films were annealed using a controlled heating/cooling apparatus. The transformations in the crystal structure were observed via in-situ synchrotron x-ray diffraction. The samples were annealed to various temperatures in the range of 400-1100° C. The onset and progression of particle formation were studied in-situ via laser measurements. In addition, a four-point probe measurement tool was used to record the changes in the resistivity of the films, which is affected by phase transformation, as well as roughening and agglomeration. Thin films annealed at various temperature steps were then studied via atomic force microscopy, scanning electron microscopy and high-resolution transmission electron microscopy, in order to get a better understanding of the correlated mechanisms, through which phase transformation and particle formation occur. The results indicate that the onset of hcp-to-bcc transformation is at 400°C, while particle formations commences at 590° C. If the annealed films are quenched after transformation, but prior to agglomeration, they show a noticeable drop in resistivity. This can be attributed to the fact that the hcp films are grown epitaxially, and are under severe tensile strain, and annealing leads to relaxation of the mismatch strain. In general, the results shed light on the nature of structural transformation in nickel thin films, as well as metallic thin films, in general.

Keywords: atomic layer deposition, metastable, nickel, phase transformation, thin film

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Authors: Aghaei Amirkhizi Navideh, Sadjadi Soodeh Sadat, Moghaddam Banaem Leila, Athari Allaf Mitra, Johari Daha Fariba

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Dendrimers are good candidates for preparing metal nanoparticles because they can structurally and chemically well-defined templates and robust stabilizers. Poly amidoamine (PAMAM) dendrimer-based multifunctional cancer therapeutic conjugates have been designed and synthesized in pharmaceutical industry. In addition, encapsulated nanoparticle surfaces are accessible to substrates so that catalytic reactions can be carried out. For preparation of dendimer-metal nanocomposite, a dendrimer solution containing an average of 55 Yb+3 ions per dendrimer was prepared. Prior to reduction, the pH of this solution was adjusted to 7.5 using NaOH. NaBH4 was used to reduce the dendrimer-encapsulated Yb+3 to the zerovalent metal. The pH of the resulting solution was then adjusted to 3, using HClO4, to decompose excess BH4-. The UV-Vis absorption spectra of the mixture were recorded to ensure the formation of Yb-G5-NH2 complex. High-resolution electron microscopy (HRTEM) and size distribution results provide additional information about dendimer-metal nanocomposite shape, size, and size distribution of the particles. The resulting mixture was irradiated in Tehran Research Reactor 2h and neutron fluxes were 3×1011 n/cm2.Sec and the specific activity was 7MBq. Radiochemical and chemical and radionuclide quality control testes were carried. Gamma Spectroscopy and High-performance Liquid Chromatography HPLC, Thin-Layer Chromatography TLC were recorded. The injection of resulting solution to solid tumor in mice shows that it could be resized the tumor. The studies about solid tumors and nano composites show that ytterbium encapsulated-dendrimer radiopharmaceutical could be introduced as a new therapeutic for the treatment of solid tumors.

Keywords: nano-radio pharmaceutical, ytterbium, PAMAM, dendrimers

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Authors: Marie Kudrnová, Jana Rejková

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The samples of supplied INCONEL 601, 617, 625, and HASTELLOY C-22 alloys and experimental nickel alloy MoNiCr were examined by XPS (X-ray photoelectron spectroscopy) before and after exposure. The experiment was performed in a mixture of LiCl-KCl salt (58.2-41.8 wt. %). The exposure conditions were 440°C, pressure 0.2 MPa, 500 hours in an inert argon atmosphere. The XPS analysis shows that a thin oxide layer composed of metal oxides such as NiO, Cr₂O₃, and Nb₂O₅ was formed. After sputtering the exposed surface with Ar ions, metals were also detected in the elemental state, indicating a very thin protective oxide layer with a thickness in units of up to tens of nanometers.

Keywords: XPS, MSR, nickel alloy, metal oxides

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Authors: Marie Kudrnova, Jana Petru

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This study is part of the international research - Materials for Molten Salt Reactors (MSR) and addresses the part of the project dealing with the corrosion behavior of candidate construction materials. Inconel 625 was characterized by x-ray photoelectron spectroscopy (XPS) before and after high–temperature experiment in molten salt. The experiment was performed in a horizontal tube furnace molten salt reactor, at 450 °C in argon, at atmospheric pressure, for 150 hours. Industrially produced HITEC salt was used (NaNO3, KNO3, NaNO2). The XPS study was carried out using the ESCAProbe P apparatus (Omicron Nanotechnology Ltd.) equipped with a monochromatic Al Kα (1486.6 eV) X-ray source. The surface layer on alloy 625 after exposure contains only Na, C, O, and Ni (as NiOx) and Nb (as NbOx BE 206.8 eV). Ni was detected in the metallic state (Ni0 – Ni 2p BE-852.7 eV, NiOx - Ni 2p BE-854.7 eV) after a short Ar sputtering because the oxide layer on the surface was very thin. Nickel oxides can form a protective layer in the molten salt, but only future long-term exposures can determine the suitability of Inconel 625 for MSR.

Keywords: Inconel 625, molten salt, oxide layer, XPS

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Authors: Jaibir Sharma, Lee JaeWung, Merugu Srinivas, Navab Singh

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This paper presents thermal annealing dewetting technique for the preparation of porous metal membrane for thin film encapsulation application. Thermal annealing dewetting experimental results reveal that pore size in porous metal membrane depend upon i.e. 1. The substrate on which metal is deposited for formation of porous metal cap membrane, 2. Melting point of metal used for porous metal cap layer membrane formation, 3. Thickness of metal used for cap layer, 4. Temperature used for porous metal membrane formation. Silver (Ag) was used as a metal for preparation of porous metal membrane by annealing the film at different temperature. Pores in porous silver film were analyzed using Scanning Electron Microscope (SEM). In order to check the usefulness of porous metal film for thin film encapsulation application, the porous silver film prepared on amorphous silicon (a-Si) was release using XeF2. Finally, guide line and structures are suggested to use this porous membrane for thin film encapsulation (TFE) application.

Keywords: dewetting, themal annealing, metal, melting point, porous

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Authors: Grigoria Athanasaki, Veerarajan Vimala, A. M. Kannan, Louis Cindrella

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Energy usage has been increased throughout the years, leading to severe environmental impacts. Since the majority of the energy is currently produced from fossil fuels, there is a global need for clean energy solutions. Proton Exchange Membrane Fuel Cells (PEMFCs) offer a very promising solution for transportation applications because of their solid configuration and low temperature operations, which allows them to start quickly. One of the main components of PEMFCs is the Gas Diffusion Layer (GDL), which manages water and gas transport and shows direct influence on the fuel cell performance. In this work, a novel dual-layer GDL with gradient porosity was prepared, using polyethylene glycol (PEG) as pore former, to improve the gas diffusion and water management in the system. The microporous layer (MPL) of the fabricated GDL consists of carbon powder PUREBLACK, sodium dodecyl sulfate as a surfactant, 34% wt. PTFE and the gradient porosity was created by applying one layer using 30% wt. PEG on the carbon substrate, followed by a second layer without using any pore former. The total carbon loading of the microporous layer is ~ 3 mg.cm-2. For the assembly of the catalyst layer, Nafion membrane (Ion Power, Nafion Membrane NR211) and Pt/C electrocatalyst (46.1% wt.) were used. The catalyst ink was deposited on the membrane via microspraying technique. The Pt loading is ~ 0.4 mg.cm-2, and the active area is 5 cm2. The sample was ex-situ characterized via wetting angle measurement, Scanning Electron Microscopy (SEM), and Pore Size Distribution (PSD) to evaluate its characteristics. Furthermore, for the performance evaluation in-situ characterization via Fuel Cell Testing using H2/O2 and H2/air as reactants, under 50, 60, 80, and 100% relative humidity (RH), took place. The results were compared to a single layer GDL, fabricated with the same carbon powder and loading as the dual layer GDL, and a commercially available GDL with MPL (AvCarb2120). The findings reveal high hydrophobic properties of the microporous layer of the GDL for both PUREBLACK based samples, while the commercial GDL demonstrates hydrophilic behavior. The dual layer GDL shows high and stable fuel cell performance under all the RH conditions, whereas the single layer manifests a drop in performance at high RH in both oxygen and air, caused by catalyst flooding. The commercial GDL shows very low and unstable performance, possibly because of its hydrophilic character and thinner microporous layer. In conclusion, the dual layer GDL with PEG appears to have improved gas diffusion and water management in the fuel cell system. Due to its increasing porosity from the catalyst layer to the carbon substrate, it allows easier access of the reactant gases from the flow channels to the catalyst layer, and more efficient water removal from the catalyst layer, leading to higher performance and stability.

Keywords: gas diffusion layer, microporous layer, proton exchange membrane fuel cells, relative humidity

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Authors: Bahattin Duzgun, Adem Kocyigit, Demet Tatar, Ahmet Battal

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Tin oxide thin films are semiconductor materials highly transparent and with high mechanical and chemical stability, except for their interactions with oxygen atoms at high temperature. Many dopants, such as antimony (Sb), arsenic (As), fluorine (F), indium (In), molybdenum and (Mo) etc. have been used to improve the electrical properties of tin oxide films. Among these, Sb and F are found to be the most commonly used dopants for solar cell layers. Also Tin oxide tin films investigated and characterized by researchers different film deposition and analysis method. In this study, tin oxide thin films are deposited on glass substrate by spin coating technique and characterized by FTIR and AFM. FTIR spectroscopy revealed that all films have O-Sn-O and Sn-OH vibration bonds not changing with layer effect. AFM analysis indicates that all films are homogeneity and uniform. It can be seen that all films have needle shape structure in their surfaces. Uniformity and homogeneity of the films generally increased for increasing layers. The results found in present study showed that doubly doped SnO2 thin films is a good candidate for solar cells and other optoelectronic and technological applications.

Keywords: doubly doped, spin coating, FTIR analysis, AFM analysis

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Authors: Nadeem A. Siddique, Mohd Mujeeb, Kahkashan

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Introduction: The objective of the projected work is to study the occurrence of the aflatoxins B1, B2, G1and G2 in remedial plants, exclusively in Delphinium denudatum. The aflatoxins were analysed by high-performance liquid chromatography–tandem quadrupole mass spectrometry with electrospray ionization (HPLC–MS/MS) and immunoaffinity column chromatography were used for extraction and purification of aflatoxins. PDA media was selected for fungal count. Results: A good quality linear relationship was originated for AFB1, AFB2, AFG1 and AFG2 at 1–10 ppb (r > 0.9995). The analyte precision at three different spiking levels was 88.7–109.1 %, by means of low per cent relative standard deviations in each case. Within 5 to7 min aflatoxins can be separated using an Agilent XDB C18-column. We found that AFB1 and AFB2 were not found in D. denudatum. This was reliable through exceptionally low figures of fungal colonies observed after 6 hr of incubation. The developed analytical method is straightforward, be successfully used to determine the aflatoxins. Conclusion: The developed analytical method is straightforward, simple, accurate, economical and can be successfully used to find out the aflatoxins in remedial plants and consequently to have power over the quality of products. The presence of aflatoxin in the plant extracts was interrelated to the least fungal load in the remedial plants examined.

Keywords: aflatoxins, delphinium denudatum, liquid chromatography, mass spectrometry

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Authors: A. Bouloufa, K. Djessas

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In this paper, we reported the effect of substrate temperature on the structural, electrical and optical properties of In2S3 thin films deposited on soda-lime glass substrates by physical vapor deposition technique at various substrate temperatures. The In2Se3 material used for deposition was synthesized from its constituent elements. It was found that all samples exhibit one phase which corresponds to β-In2S3 phase. Values of band gap energy of the films obtained at different substrate temperatures vary in the range of 2.38-2.80 eV and decrease with increasing substrate temperature.

Keywords: buffer layer, In2S3, optical properties, PVD, structural properties

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Authors: Xavier A. Conlan

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Speed of analysis is a significant limitation to current high-performance liquid chromatography/mass spectrometry (HPLC/MS) and ultra-high-pressure liquid chromatography (UHPLC)/MS systems both of which are used in many forensic investigations. The flow rate limitations of MS detection require a compromise in the chromatographic flow rate, which in turn reduces throughput, and when using modern columns, a reduction in separation efficiency. Commonly, this restriction is combated through the post-column splitting of flow prior to entry into the mass spectrometer. However, this results in a loss of sensitivity and a loss in efficiency due to the post-extra column dead volume. A new chromatographic column format known as 'parallel segmented flow' involves the splitting of eluent flow within the column outlet end fitting, and in this study we present its application in order to interrogate the provenience of methamphetamine samples with mass spectrometry detection. Using parallel segmented flow, column flow rates as high as 3 mL/min were employed in the analysis of amino acids without post-column splitting to the mass spectrometer. Furthermore, when parallel segmented flow chromatography columns were employed, the sensitivity was more than twice that of conventional systems with post-column splitting when the same volume of mobile phase was passed through the detector. These finding suggest that this type of column technology will particularly enhance the capabilities of modern LC/MS enabling both high-throughput and sensitive mass spectral detection.

Keywords: chromatography, mass spectrometry methamphetamine, parallel segmented outlet flow column, forensic sciences

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Authors: Yifan Gao

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Owing to the high breakdown field, high saturation drift velocity, 2DEG with high density and mobility and so on, AlGaN/GaN HEMTs have been widely used in high-frequency and high-power applications. To acquire a higher power often means higher breakdown voltage and higher drain current. Surface leakage current is usually the key issue affecting the breakdown voltage and power performance. In this work, we have performed in-situ N₂/NH₃ pretreatment before the passivation to suppress the surface leakage and achieve device performance enhancement. The AlGaN/GaN HEMT used in this work was grown on a 3-in. SiC substrate, whose epitaxial structure consists of a 3.5-nm GaN cap layer, a 25-nm Al₀.₂₅GaN barrier layer, a 1-nm AlN layer, a 400-nm i-GaN layer and a buffer layer. In order to analyze the mechanism for the N-based pretreatment, the details are measured by XPS analysis. It is found that the intensity of Ga-O bonds is decreasing and the intensity of Ga-N bonds is increasing, which means with the supplement of N, the dangling bonds on the surface are indeed reduced with the forming of Ga-N bonds, reducing the surface states. The surface states have a great influence on the leakage current, and improved surface states represent a better off-state of the device. After the N-based pretreatment, the breakdown voltage of the device with Lₛ𝒹=6 μm increased from 93V to 170V, which increased by 82.8%. Moreover, for HEMTs with Lₛ𝒹 of 6-μm, we can obtain a peak output power (Pout) of 12.79W/mm, power added efficiency (PAE) of 49.84% and a linear gain of 20.2 dB at 60V under 3.6GHz. Comparing the result with the reference 6-μm device, Pout is increased by 16.5%. Meanwhile, PAE and the linear gain also have a slight increase. The experimental results indicate that using N₂/NH₃ pretreatment before passivation is an attractive approach to achieving power performance enhancement.

Keywords: AlGaN/GaN HEMT, N-based pretreatment, output power, passivation

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Authors: Suhas Kadam, Vishal Chandanshive, Niraj Rane, Sanjay Govindwar

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Fimbristylis dichotoma, Ammannia baccifera, and their co-plantation consortium FA were found to degrade methyl orange, simulated dye mixture, and real textile effluent. Wild plants of Fimbristylis dichotoma and Ammannia baccifera with equal biomass showed 91 and 89% decolorization of methyl orange within 60 h at a concentration of 50 ppm, while 95% dye removal was achieved by consortium FA within 48 h. Floating phyto-beds with co-plantation (Fimbristylis dichotoma and Ammannia baccifera) for the treatment of real textile effluent in a constructed wetland was observed to be more efficient and achieved 79, 72, 77, 66 and 56% reductions in ADMI color value, chemical oxygen demand, biological oxygen demand, total dissolve solid and total suspended solid of textile effluent, respectively. High performance thin layer chromatography, gas chromatography-mass spectroscopy, Fourier transform infrared spectroscopy, Ultra violet-Visible spectroscopy and enzymatic assays confirmed the phytotransformation of parent dye in the new metabolites. T-RFLP analysis of rhizospheric bacteria of Fimbristylis dichotoma, Ammannia baccifera, and consortium FA revealed the presence of 88, 98 and 223 genera which could have been involved in dye removal. Toxicity evaluation of products formed after phytotransformation of methyl orange by consortium FA on bivalves Lamellidens marginalis revealed less damage in the gills architecture when analyzed histologically. Toxicity measurement by Random Amplification of Polymorphic DNA (RAPD) technique revealed normal banding pattern in treated methyl orange sample suggesting less toxic nature of phytotransformed dye products.

Keywords: constructed wetland, phyto-bed, textile effluent, phytoremediation

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Authors: Preeti Panthari, Harsha Kharkwal

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Myrica nagi belongs to Myricaceae family. It is known for its therapeutic use since ancient times. The leaves were extracted with methanol and further fractioned with different solvents with increasing polarity. The n-butanol fraction of methanol extract was passed through celite, on separation through silica gel column chromatography yielded ten fractions. For the first time we report isolation of Caffeic acid from n-butanol fraction of Myrica nagi leaves in Chloroform: methanol (70:30) fraction. The mobile phase used for analysis in HPLC was Methanol: water (60:40) at the flow rate of 1 ml/min at wavelength of 280 nm. The retention time was 2.66 mins.

Keywords: Myrica nagi, column chromatography, retention time, caffeic acid

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Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

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Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

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Authors: Hamid Merzouk, Dajhida Talantikite, Amel Tounsi

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Thin films of ZnS have been deposited by chemical route into acidic medium. The deposition time fixed at 5 hours, and the bath temperature varied from 80° C to 95°C with an interval of 5°C. The X-ray diffraction (XRD), UV/ visible spectrophotometry, Fourier Transform Infrared spectroscopy (FTIR) have been used to study the effect of temperature on the structural and optical properties of ZnS thin films. The XRD spectrum of the ZnS layer obtained shows an increase of peaks intensity of ZnS with increasing bath temperature. The study of optical properties exhibit good transmittance (60–80% in the visible region), and the band gap energy of the ZnS thin film decrease from 3.71 eV to 3.64 eV while the refractive index (n) increase with increasing temperature bath. The FTIR analyze confirm our studies and show characteristics bands of vibration of Zn-S.

Keywords: ZnS thin films, XRD spectra, optical gap, XRD

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Authors: Ali H. Mahfouz, Hossam E. M. Sallam, Abdulwali Wazir, Hamod H. Kharezi

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The soil profile at site of the bridge project includes soft fine grained soil layer located between 5.0 m to 11.0 m in depth, it has high water content, low SPT no., and low bearing capacity. The clay layer induces high settlement due to surcharge application of earth embankment at ramp T1, ramp T2, and ramp T3 especially at heights from 9m right 3m. Calculated settlement for embankment heights less than 3m may be accepted regarding Saudi Code for soil and foundation. The soil and groundwater at the project site comprise high contents of sulfates and chlorides of high aggressively on concrete and steel bars, respectively. Regarding results of the study, it has been recommended to use stone column piles or new technology named PCC piles as soil improvement to improve the bearing capacity of the weak layer. The new technology is cast in-situ thin wall concrete pipe piles (PCC piles), it has economically advantageous and high workability. The technology can save time of implementation and cost of application is almost 30% of other types of piles.

Keywords: soft foundation soil, bearing capacity, bridge ramps, soil improvement, geogrid, PCC piles

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Authors: M. H. Aldahrob, A. Kokce, S. Altindal, H. E. Lapa

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In order to obtain the detailed information about the effect of (Zn-doped PVA) interfacial layer, surface states (Nss) and series resistance (Rs) on electrical characteristics, both Au/n- type 4H-SiC (MS) with and without (Zn doped PVA) interfacial layer were fabricated to compare. The main electrical parameters of them were investigated using forward and reverse bias current-voltage (I-V), capacitance-voltage (C-V) and conductance –voltage (G/W –V) measurements were performed at room temperature. Experimental results show that the value of ideality factor (n), zero –bias barrier height (ΦBo), Rs, rectifier rate (RR=IF/IR) and the density of Nss are strong functions interfacial layer and applied bias voltage. The energy distribution profile of Nss was obtained from forward bias I-V data by taking into account voltage dependent effective BH (ΦBo) and ideality factor (n(V)). Voltage dependent profile of Rs was also obtained both by using Ohm’s law and Nicollian and Brew methods. The other main diode parameters such as the concentration of doping donor atom (ND), Fermi energy level (EF).BH (ΦBo), depletion layer with (WD) were obtained by using the intercept and slope of the reverse bias C-2 vs V plots. It was found that (Zn-doped PVA) interfacial layer lead to a quite decrease in the values Nss, Rs and leakage current and increase in shunt resistance (Rsh) and RR. Therefore, we can say that the use of thin (Zn-doped PVA) interfacial layer can quite improved the performance of MS structure.

Keywords: interfacial polymer layer, thickness dependence, electric and dielectric properties, series resistance, interface state

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Authors: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

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In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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Authors: Sari F. Alkhatib, Chang Je Park, Gyuhong Roh

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The iterative scheme which is used to treat buildup factors for stratified shields is being investigated here using the layer-splitting technique. A simple suggested formalism for the scheme based on the Kalos’ formula is introduced, based on which the implementation of the testing technique is carried out. The second layer in a double-layer shield was split into two equivalent layers and the scheme (with the suggested formalism) was implemented on the new “three-layer” shield configuration. The results of such manipulation on water-lead and water-iron shields combinations are presented here for 1 MeV photons. It was found that splitting the second layer introduces some deviation on the overall buildup factor value. This expected deviation appeared to be higher in the case of low Z layer followed by high Z. However, the overall performance of the iterative scheme showed a great consistency and strong coherence even with the introduced changes. The introduced layer-splitting testing technique shows the capability to be implemented in test the iterative scheme with a wide range of formalisms.

Keywords: buildup factor, iterative scheme, stratified shields, layer-splitting tecnique

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Authors: Ruchi B. Semwal, Deepak K. Semwal, Thobile A. N. Nkosi, Alvaro M. Viljoen

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The use of Lawsonia inermis L. (Lythraeae), commonly known as henna, has many medicinal benefits and is used as a remedy for the treatment of diarrhoea, cancer, inflammation, headache, jaundice and skin diseases in folk medicine. Although widely used for hair dyeing and temporary tattooing, henna body art has popularized over the last 15 years and changed from being a traditional bridal and festival adornment to an exotic fashion accessory. The naphthoquinone, lawsone, is one of the main constituents of the plant and responsible for its dyeing property. Henna leaves typically contain 1.8–1.9% lawsone, which is used as a marker compound for the quality control of henna products. Adulteration of henna with various toxic chemicals such as p-phenylenediamine, p-methylaminophenol, p-aminobenzene and p-toluenodiamine to produce a variety of colours, is very common and has resulted in serious health problems, including allergic reactions. This study aims to assess the quality of henna products collected from different parts of the world by determining the lawsone content, as well as the concentrations of any adulterants present. Ultra high performance liquid chromatography-mass spectrometry (UPLC-MS) was used to determine the lawsone concentrations in 172 henna products. Separation of the chemical constituents was achieved on an Acquity UPLC BEH C18 column using gradient elution (0.1% formic acid and acetonitrile). The results from UPLC-MS revealed that of 172 henna products, 11 contained 1.0-1.8% lawsone, 110 contained 0.1-0.9% lawsone, whereas 51 samples did not contain detectable levels of lawsone. High performance thin layer chromatography was investigated as a cheaper, more rapid technique for the quality control of henna in relation to the lawsone content. The samples were applied using an automatic TLC Sampler 4 (CAMAG) to pre-coated silica plates, which were subsequently developed with acetic acid, acetone and toluene (0.5: 1.0: 8.5 v/v). A Reprostar 3 digital system allowed the images to be captured. The results obtained corresponded to those from UPLC-MS analysis. Vibrational spectroscopy analysis (MIR or NIR) of the powdered henna, followed by chemometric modelling of the data, indicates that this technique shows promise as an alternative quality control method. Principal component analysis (PCA) was used to investigate the data by observing clustering and identifying outliers. Partial least squares (PLS) multivariate calibration models were constructed for the quantification of lawsone. In conclusion, only a few of the samples analysed contain lawsone in high concentrations, indicating that they are of poor quality. Currently, the presence of adulterants that may have been added to enhance the dyeing properties of the products, is being investigated.

Keywords: Lawsonia inermis, paraphenylenediamine, temporary tattooing, lawsone

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Authors: Sudhanshu Sharma

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Lisinopril, 1-[N-{(s)-I-carboxy-3 phenyl propyl}-L-proline dehydrate is a lysine analog of enalaprilat, the active metabolite of enalapril. It is long-acting, non-sulhydryl angiotensin-converting enzyme (ACE) inhibitor that is used for the treatment of hypertension and congestive heart failure in daily dosage 10-80 mg. Pharmacological activity of lisinopril has been proved in various experimental and clinical studies. Owing to its importance and widespread use, efforts have been made towards the development of simple and reliable analytical methods. As per our literature survey, lisinopril in pharmaceutical formulations has been determined by various analytical methodologies like polaragraphy, potentiometry, and spectrophotometry, but most of these analytical methods are not too suitable for the Identification of lisinopril from clinical samples because of the interferences caused by the amino acids and amino groups containing metabolites present in biological samples. This report is an attempt in the direction of developing a simple and reliable method for on plate identification and quantification of lisinopril in pharmaceutical formulations as well as from human urine samples using silica gel H layers developed with a new mobile phase comprising of micellar solutions of N-cetyl-N, N, N-trimethylammonium bromide (CTAB). Micellar solutions have found numerous practical applications in many areas of separation science. Micellar liquid chromatography (MLC) has gained immense popularity and wider applicability due to operational simplicity, cost effectiveness, relatively non-toxicity and enhanced separation efficiency, low aggressiveness. Incorporation of aqueous micellar solutions as mobile phase was pioneered by Armstrong and Terrill as they accentuated the importance of TLC where simultaneous separation of ionic or non-ionic species in a variety of matrices is required. A peculiarity of the micellar mobile phases (MMPs) is that they have no macroscopic analogues, as a result the typical separations can be easily achieved by using MMPs than aqueous organic mobile phases. Previously MMPs were successfully employed in TLC based critical separations of aromatic hydrocarbons, nucleotides, vitamin K1 and K5, o-, m- and p- aminophenol, amino acids, separation of penicillins. The human urine analysis for identification of selected drugs and their metabolites has emerged as an important investigation tool in forensic drug analysis. Among all chromatographic methods available only thin layer chromatography (TLC) enables a simple fast and effective separation of the complex mixtures present in various biological samples and is recommended as an approved testing for forensic drug analysis by federal Law. TLC proved its applicability during successful separation of bio-active amines, carbohydrates, enzymes, porphyrins, and their precursors, alkaloid and drugs from urine samples.

Keywords: lisnopril, surfactant, chromatography, micellar solutions

Procedia PDF Downloads 339

Authors: Qiao Pei Wen, Ng Seng Lee, Sae Tae Veera, Chiu Ah Fong, Loke Weng Onn

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Thin film thickness uniformity is crucial to get consistent film etch rate and device yield across the wafer. In the capacitive-coupled parallel plate PECVD system; the film thickness uniformity can be affected by many factors such as the heater temperature uniformity, the spacing between top and bottom electrode, RF power, pressure, gas flows and etc. In this paper, we studied how the PECVD SiN film thickness uniformity is affected by the substrate electrical conductivity and the RF power coupling efficiency. PECVD SiN film was deposited on 150-mm sapphire wafers in 200-mm Lam Sequel tool, fork marks were observed on the wafers. On the fork marks area SiN film thickness is thinner than that on the non-fork area. The forks are the wafer handler inside the process chamber to move the wafers from one station to another. The sapphire wafers and the ceramic forks both are insulator. The high resistivity of the sapphire wafers and the forks inhibits the RF power coupling efficiency during PECVD deposition, thereby reducing the deposition rate. Comparing between the high frequency and low frequency RF power (HFRF and LFRF respectively), the LFRF power coupling effect on the sapphire wafers is more dominant than the HFRF power on the film thickness. This paper demonstrated that the SiN thickness uniformity on sapphire wafers can be improved by depositing a thin TiW layer on the wafer before the SiN deposition. The TiW layer can be on the wafer surface, bottom or any layer before SiN deposition.

Keywords: PECVD SiN deposition, sapphire wafer, substrate electrical conductivity, RF power coupling, high frequency RF power, low frequency RF power, film deposition rate, thickness uniformity

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Authors: Špela Hajduk, Sean P. Berglund, Matejka Podlogar, Goran Dražić, Fatwa F. Abdi, Zorica C. Orel, Menny Shalom

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Graphitic carbon nitride materials (g-CN) have emerged as an attractive photocatalyst and electrocatalyst for photo and electrochemical water splitting reaction, due to their environmental benignity nature and suitable band gap. Many approaches were introduced to enhance the photoactivity and electronic properties of g-CN and resulted in significant changes in the electronic and catalytic properties. Here we demonstrate the synthesis of thin and homogenous g-CN layer on highly ordered ZnO nanowire (NW) substrate by growing a seeding layer of small supramolecular assemblies on the nanowires. The new synthetic approach leads to the formation of thin g-CN layer (~3 nm) without blocking all structure. Two different deposition methods of carbon nitride were investigated and will be presented. The amount of loaded carbon nitride significantly influences the PEC activity of hybrid material and all the ZnO/g-CNx electrodes show great improvement in photoactivity. The chemical structure, morphology and optical properties of the deposited g-CN were fully characterized by various techniques as X-ray powder spectroscopy (XRD), scanning electron microscopy (SEM), focused ion beam scanning electron microscopy (FIB-SEM), high-resolution scanning microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS).

Keywords: carbon nitride, photoanode, solar water splitting, zinc oxide

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Authors: Huda Aldossari

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Members of the Brassicaceae family, such as rocket species, have high concentrations of glucosinolates (GLSs). GSLs and isothiocyanates (ITCs), the product of GLSs hydrolysis, are the most influential compounds that affect flavour in rocket species. Aside from their contribution to the flavour, GSLs and ITCs are of particular interest due to their potential ability to inhibit the growth of human pathogenic bacteria such as E. coli O157. Quantitative and qualitative analysis of glucosinolate compounds in rocket extracts was obtained by Liquid Chromatography-Mass Spectrometry (LC–MS).Each individual component of non-volatile GLSs and ITCs was isolated by High-Performance Liquid Chromatography (HPLC) fractionation. The identity and purity of each fraction were confirmed using Ultra High-Performance Liquid Chromatography (UPLC). The separation of glucosinolates in the complex rocket extractions was performed by optimizing a HPLC fractionation method through changing the mobile phase composition, solvent gradient, and the flow rate. As a result, six glucosinolates compounds (Glucosativin, 4-Methoxyglucobrassicin, Glucotropaeolin GTP, Glucoiberin GIB, Diglucothiobenin, and Sinigrin) have been isolated, identified and quantified in the complex samples. This step aims to evaluate the antibacterial activity of glucosinolates and their enzymatic hydrolysis against bacterial growth of E.coli k12. Therefore, fractions from this study will be used to determine the most active compounds by investigating the efficacy of each component of GLSs and ITCs at inhibiting bacterial growth.

Keywords: rocket, glucosinolates, E.coli k12., HPLC fractionatio

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Authors: Kang Jian Xian, Huda Abdullah, Md. Akhtaruzzaman, Iskandar Yahya, Mohd Hafiz Dzarfan Othman, Brian Yulianto

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The CZTS absorber layer doped with a silver (Ag) is one of the candidates that suggest improving the efficiency of thin films. Silver element functions to reduce antisite defects, increase grain size and create the plasmonic effect. In this work, an experimental study has been done to investigate the electrical and physical properties of CZTS, ACZTS, and AZTS. Ag replaces the Cu in (Cu1-xAgx)2ZnSnS4 (ACZTS) is up to x ≤1. ACZTS thin-films solar cells have been deposited by sol–the gel spin coating method. There are a total of 19 samples done with 11 significant percentages (0%, 10%, 20%… 100%) to show the whole phenomena of efficiency rate and nine specific percentages to find out the best concentration rate for Ag-doped. The obtained results can be helpful for better understanding ACZTS layers.

Keywords: CZTS, ACZTS, AZTS, silver, antisite, efficiency, thin-film solar cell

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