Search results for: ultrafast laser spectroscopy

Authors: N. Tugrul, F. T. Senberber, A. S. Kipcak, E. Moroydor Derun, S. Piskin

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In this research, it is aimed not only microwave synthesis of magnesium borates but also evaluation of magnesium wastes. Synthesis process can be described with the reaction of Mg wastes and boric acid using microwave energy. X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied to synthesized minerals. According to XRD results, magnesium borate hydrate mixtures were obtained as mcallisterite (pdf# = 01-070-1902, Mg2(B6O7(OH)6)2.9(H2O)) at higher crystallinity properties was achieved at the mole ratio raw material 1:1. Also, other kinds of magnesium borate hydrates were obtained at lower crystallinity such as admontite (pdf # = 01-076-0540, MgO(B2O3)3.7(H2O)), inderite (pdf # = 01-072-2308, 2MgO.3B2O3.15(H2O)) and magnesium borate hydrates (pdf # = 01-076-0539, MgO(B2O3)3.6(H2O)). FT-IR spectrums indicated that minor changes were seen at the band values of characteristic stretching in each experiment. At the end of experiments it is seen that using microwave energy may contribute positive effects to design of synthesis process such as reducing reaction time and products at higher crystallinity.

Keywords: magnesium wastes, boric acid, magnesium borate, microwave energy

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Authors: Dalila Hocine, Mohammed Said Belkaid, Abderahmane Moussi

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In this study, pure rutile TiO2 thin films were directly synthesized on silicon substrates by Atmospheric Pressure Chemical Vapor Deposition technique (APCVD) using TiCl4 as precursor. We studied the physicochemical properties and the optical properties of the produced coatings by means of standard characterization techniques of Fourier Transform Infrared Spectroscopy (FTIR) combined with UV-Vis Reflectance Spectrophotometry. The absorption peaks at 423 cm-1 and 610 cm-1 were observed for the rutile TiO2 thin films, by FTIR measurements. The absorption peak at 739 cm-1 due to the vibration of the Ti-O bonds, was also detected. UV-Vis Reflectance Spectrophotometry is employed for measuring the optical band gap from the measurements of the TiO2 films reflectance. The optical band gap was then extracted from the reflectance data for the TiO2 sample. It was estimated to be 3.05 eV which agrees with the band gap of commercial rutile TiO2 sample.

Keywords: titanium dioxide, physicochemical properties, APCVD, FTIR, band gap

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Authors: Vishakha Parihar

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This study reports the preparation of iron metal-doped nanoparticles of Titanium dioxide by the sol-gel process and the photocatalytic degradation of dye. Nano-particles were characterized by SEM, EDX, and UV-Vis spectroscopy. The detailed study confirmed that nanoparticles have grown in high density and have good optical properties. The photocatalytic batch experiment was performed in an aqueous solution where congo red dye was used as a dye pollutant under the irradiation of ultraviolet rays created by using a mercury lamp source. Total degradation efficiency achieved was approximately 85% to 93% in the duration of 100-120 minutes of irradiation under an ultraviolet light source. The decolorization ability of this process was measured by absorbance at a maximum wavelength of 498nm. The results indicated that the iron-doped Titanium dioxide nanoparticles showed an excellent photocatalytic response to the degradation of dye under the ultraviolet light source within a very short period of time.

Keywords: titanium dioxide, nano-particles iron dope, photocatalytic degradation, Congo red dye, sol-gel process

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Authors: Faroojan Khajeek Sisak Siakian, Aayda Dikran Abdulahad

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The Peris Mountain is one of the main mountains in the Iraqi Kurdistan Region, it forms one of the long anticlines trending almost East – West. The exposed formations on the top of the mountain are Bekhme, and Shiranish, with carbonate rocks of different types and thicknesses. We selected the site for sampling to be relevant for a quarry taking into consideration the thickness of the exposed rocks, no overburden, favorable quarrying faces, hardness of the rocks, bedding nature, good extension of the outcrops, and a favorable place for construction of a cement plant. We sampled the exposed rocks on the top of the mountain where a road crosses the mountain, and a total of 15 samples were collected. The distance between sampling intervals was 5 m, and each sample was collected to represent the sampling interval. The samples were subjected to X-ray fluorescence spectroscopy (XRF) to indicate the main oxides percentages in each sample. The acquired results showed the studied rocks can be used in the cement industry.

Keywords: limestone, quarry, CaO, MgO, overburden

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Authors: Catalin Croitoru, Ionut Claudiu Roata

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Employing concentrated solar energy (CSE) for sintering metallic parts offers distinct advantages, notably in the rapid thermal cycling that significantly influences their microstructure and phase transitions. This study uses the thermal control that CSE affords, enhancing the mechanical properties and tailoring the functionality of nickel-based alloys. We synthesized bulk alloys by sintering Ni-Cr-Al-Y powders in varied ratios using a vertical solar furnace at PROMES-CNRS, Font-Romeu Odeillo, France. The process achieved optimal fusion at 800°C for 10 minutes, resulting in materials with a notable hydrophilic surface due to oxide formation. The alloys’ performance was evaluated through corrosion resistance tests in a 3.5% wt. NaCl solution, utilizing potentiodynamic scanning and electrochemical impedance spectroscopy. Our findings demonstrate the potential of CSE in advancing the material properties of nickel-based alloys for diverse applications.

Keywords: concentrated solar energy, sintering, corrosion resistance, surface properties

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Authors: Mohamed A. Deyab, Ahmed E. Awadallah

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Under various conditions, we present a promising method for producing pure hydrogen energy from the electrochemical reaction of Mg metal in waste oilfield water (WOW). Mg metal and WOW are primarily consumed in this process. The results show that the hydrogen gas output is highly dependent on temperature and solution pH. The best conditions for hydrogen production were found to be a low pH (2.5) and a high temperature (338 K). For the first time, the Allyl methylimidazolium bis-trifluoromethyl sulfonyl imide) (IL) ionic liquid is used to regulate the rate of hydrogen generation. It has been confirmed that increasing the solution temperature and decreasing the solution pH accelerates Mg dissolution and produces more hydrogen per unit of time. The adsorption of IL on the active sites of the Mg surface is unrestricted by mixing physical and chemical orientation. Inspections using scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and FT-IR spectroscopy were used to identify and characterise surface corrosion of Mg in WOW. This process is also completely safe and can create energy on demand.

Keywords: hydrogen production, Mg, wastewater, ionic liquid

Procedia PDF Downloads 158

Authors: Waqas A. Toor, Anis U. Baig, Nuaman Shafqat, Raafia Irfan, Muhammad Ashraf

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A 2.45GHz microwave plasma system and its few applications have been developed. Argon and helium plasma is produced by metallic nozzle and also in a quartz tube at atmospheric pressure, using WR-340 waveguide and its tapered version. The waveguide applicator is also simulated in HFSS and field patterns are analyzed for maximum power absorption in the load. The system is tuned to operate at less than 10% reflected power. Various experimental techniques are used to initiate and sustain the plasma at atmospheric pressure. Plasma of atmospheric air is also produced without using any other shielding gas. The plasma flame is also characterized by its spectrum. Spectral analyses of plasma flame can be used for online analysis of combustion gases produced in industry. The applications of the system include glass and quartz processing, vitrification, emission spectroscopy, plasma coating. Low pressure plasma applications of the system include intense UV light for water purification and ozone generation.

Keywords: HFSS high frequency structure simulator, Microwave plasma, UV ultraviolet, WR rectangular waveguide

Procedia PDF Downloads 271

Authors: Shailendra Kumar, Lokesh Kashyap, Puneet Khanna, Nishant Patel, Rakesh Kumar, Arshad Ayub, Kelika Prakash, Yudhyavir Singh, Krithikabrindha V.

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Introduction: Spinal anesthesia is considered a standard anesthesia technique for caesarean delivery. The incidence of spinal hypotension during caesarean delivery is 70 -80%. Spinal hypotension may cause cerebral hypoperfusion in the mother, but physiologically cerebral autoregulatory mechanisms accordingly prevent cerebral hypoxia. Cerebral blood flow remains constant in the 50-150 mmHg of Cerebral Perfusion Pressure (CPP) range. Near-infrared spectroscopy (NIRS) is a non-invasive technology that is used to detect Cerebral Desaturation Events (CDEs) immediately compared to other conventional intraoperative monitoring techniques. Objective: The primary aim of the study is to correlate the change in cerebral oxygen saturation using NIRS with respect to a fall in mean blood pressure after spinal anaesthesia and to find out the effects of spinal hypotension on neonatal APGAR score, neonatal acid-base variations, and presence of Postoperative Delirium (POD). Methodology: NIRS sensors were attached to the forehead of all the patients, and their baseline readings of cerebral oxygenation on the right and left frontal regions and mean blood pressure were noted. Subarachnoid block was given with hyperbaric 0.5% bupivacaine plus fentanyl, the dose being determined by the individual anaesthesiologist. Co-loading of IV crystalloid solutions was given to the patient. Blood pressure reading and cerebral saturation were recorded every 1 minute till 30min. Hypotension was a fall in MAP less than 20% of the baseline values. Patients going for hypotension were treated with an IV Bolus of phenylephrine/ephedrine. Umbilical cord blood samples were taken for blood gas analysis, and neonatal APGAR was noted by a neonatologist. Study design: A prospective observational study conducted in a population of Thirty ASA 2 and 3 parturients scheduled for lower segment caesarean section (LSCS). Results: Mean fall in regional cerebral saturation is 28.48 ± 14.7% with respect to the mean fall in blood pressure 38.92 ± 8.44 mm Hg. The correlation coefficient between fall in saturation and fall in mean blood pressure is 0.057, and p-value {0.7} after subarachnoid block. A fall in regional cerebral saturation occurred 2±1 min before a fall in mean blood pressure. Twenty-nine out of thirty patients required vasopressors during hypotension. The first dose of vasopressor requirement is needed at 6.02±2 min after the block. The mean APGAR score was 7.86 and 9.74 at 1 and 5 min of birth, respectively, and the mean umbilical arterial pH of 7.3±0.1. According to DRS-98 (Delirium Rating Scale), the mean delirium rating score on postoperative day 1 and day 2 were 0.1 and 0.7, respectively. Discussion: There was a fall in regional cerebral oxygen saturation, which started before with respect to a significant fall in mean blood pressure readings but was statistically not significant. Maximal fall in blood pressure requiring vasopressors occurs within 10 min of SAB. Neonatal APGAR scores and acid-base variations were in the normal range with maternal hypotension, and there was no incidence of postoperative delirium in patients with post-spinal hypotension.

Keywords: cerebral oxygenation, LSCS, NIRS, spinal hypotension

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Authors: Khusboo Agrawal, S. Saraf

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Quercetin, a flavonol provides a cellular protection against UV induced oxidative damages due to its excellent free radical scavenging activity and direct pro-apoptopic effect on tumor cells. However, its topical use is limited due to its unfavorable physicochemical properties. The present study was aimed to evaluate the potential of mesoporous silica nanoparticles as topical carrier system for quercetin delivery. Complexes of quercetin with mesoporous silica was prepared with different weight ratios and characterized by thermo gravimetric analysis, X-ray diffraction, high resolution TEM, FT-IR spectroscopy, zeta potential measurements and differential scanning calorimetry The protective effect of this vehicle on UV-induced degradation of the quercetin was investigated revealing a certain positive influence of the inclusion on the photostability over time. Epidermal accumulation and transdermal permeation of this molecule were ex vivo evaluated by using Franz diffusion cells. The immobilization of Quercetin in mesoporous silica nanoparticles (MSNs) increased the stability without undermining the antioxidant efficacy.

Keywords: cancer, MSNs, quercetin, topical delivery

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Authors: Tian-Fang Kang, Chao-Nan Ge, Rui Li

Abstract:

An electrochemical biosensor for the determination of organophosphorus pesticides was developed based on electrochemical co-deposition of Au and Pd nanoparticles on glassy carbon electrode (GCE). Energy disperse spectroscopy (EDS) analysis was used for characterization of the surface structure. Scanning electron micrograph (SEM) demonstrates that the films are uniform and the nanoclusters are homogeneously distributed on the GCE surface. Acetylcholinesterase (AChE) was immobilized on the Au and Pd nanoparticle modified electrode (Au-Pd/GCE) by cross-linking with glutaraldehyde. The electrochemical behavior of thiocholine at the biosensor (AChE/Au-Pd/GCE) was studied. The biosensors exhibited substantial electrocatalytic effect on the oxidation of thiocholine. The peak current of linear scan voltammetry (LSV) of thiocholine at the biosensor is proportional to the concentration of acetylthiocholine chloride (ATCl) over the range of 2.5 × 10-6 to 2.5 × 10-4 M in 0.1 M phosphate buffer solution (pH 7.0). The percent inhibition of acetylcholinesterase was proportional to the logarithm of parathion concentration in the range of 4.0 × 10-9 to 1.0 × 10-6 M. The detection limit of parathion was 2.6 × 10-9 M. The proposed method exhibited high sensitivity and good reproducibility.

Keywords: acetylcholinesterase, Au-Pd nanoparticles, electrochemical biosensors, parathion

Procedia PDF Downloads 407

Authors: Z. Yousefniayejahr, S. Bolognini, A. Bonini, C. Campobasso, N. Poma, F. Vivaldi, M. Di Luca, A. Tavanti, F. Di Francesco

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Pathogenic bacteria represent a threat to healthcare systems and the food industry because their rapid detection remains challenging. Electrochemical biosensors are gaining prominence as a novel technology for the detection of pathogens due to intrinsic features such as low cost, rapid response time, and portability, which make them a valuable alternative to traditional methodologies. These sensors use biorecognition elements that are crucial for the identification of specific bacteria. In this context, bacteriophages are promising tools for their inherent high selectivity towards bacterial hosts, which is of fundamental importance when detecting bacterial pathogens in complex biological samples. In this study, we present the development of a low-cost and portable sensor based on the Zeno phage for the rapid detection of Staphylococcus aureus. Screen-printed gold electrodes functionalized with the Zeno phage were used, and electrochemical impedance spectroscopy was applied to evaluate the change of the charge transfer resistance (Rct) as a result of the interaction with S. aureus MRSA ATCC 43300. The phage-based biosensor showed a linear range from 101 to 104 CFU/mL with a 20-minute response time and a limit of detection (LOD) of 1.2 CFU/mL under physiological conditions. The biosensor’s ability to recognize various strains of staphylococci was also successfully demonstrated in the presence of clinical isolates collected from different geographic areas. Assays using S. epidermidis were also carried out to verify the species-specificity of the phage sensor. We only observed a remarkable change of the Rct in the presence of the target S. aureus bacteria, while no substantial binding to S. epidermidis occurred. This confirmed that the Zeno phage sensor only targets S. aureus species within the genus Staphylococcus. In addition, the biosensor's specificity with respect to other bacterial species, including gram-positive bacteria like Enterococcus faecium and the gram-negative bacterium Pseudomonas aeruginosa, was evaluated, and a non-significant impedimetric signal was observed. Notably, the biosensor successfully identified S. aureus bacterial cells in a complex matrix such as a nasal swab, opening the possibility of its use in a real-case scenario. We diluted different concentrations of S. aureus from 108 to 100 CFU/mL with a ratio of 1:10 in the nasal swap matrices collected from healthy donors. Three different sensors were applied to measure various concentrations of bacteria. Our sensor indicated high selectivity to detect S. aureus in biological matrices compared to time-consuming traditional methods, such as enzyme-linked immunosorbent assay (ELISA), polymerase chain reaction (PCR), and radioimmunoassay (RIA), etc. With the aim to study the possibility to use this biosensor to address the challenge associated to pathogen detection, ongoing research is focused on the assessment of the biosensor’s analytical performances in different biological samples and the discovery of new phage bioreceptors.

Keywords: electrochemical impedance spectroscopy, bacteriophage, biosensor, Staphylococcus aureus

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Authors: S. Gvazava, N. Khidasheli, V. Tediashvili, M. Donadze

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The work presented in this paper studied the of austempered ductile iron (ADI) with different combinations of structural composition (upper bainite, lower bainite, retained austenite) in rainwater. A range of structural states of the metal matrix was obtained by changing the regimes of thermal treantments of a high-strength cast iron. The specimens were austenised at 900 0C for 30, 60, 90, 120 minutes. Afterwards, isothermal quenching was performed at 280 and 400 0C for40 seconds. The study was carried out using weight-change (WC), cyclic potentiodynamic polarization (CPP), open-circuit potential (OCP), and electrochemical impedance spectroscopy (EIS) measurements and complemented by scanning electron microscopy (SEM-EDS). According to the results, corrosion resistance of the boron microallyedbainitic ADI greatly depends on the type of the bainitic matrix and the amount of the retained austenite, which is driven by diffusion permeability of interphase and intergrain boundaries.

Keywords: austempered ductile iron, corrosion behaviour, retained austenite, corrosion rate, interphase boundary, upper bainite, lower bainite

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Authors: Rami Al Jafar, Paul Elliott, Konstantinos K. Tsilidis, Abbas Dehghan

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Although Ramadan fasting is a ritual that is practiced every year by millions of Muslims, studies on Ramadan fasting are still scarce. To the best of our knowledge, none of the previous studies comprehensively explored the effect on the metabolic profile. In London Ramadan Fasting Study, blood samples were collected from 81 participants before and 10-14 days after Ramadan. Blood samples were analysed using nuclear magnetic resonance (NMR) spectroscopy which covers 249 metabolites. Mixed-effects models were used to analyse collected data and assess the effect of Ramadan fasting on the metabolic profile. Our observational study involved 85 individuals with a mean age of 45.2 years, and 53.1% of them were males. After Ramadan, forty metabolites were affected significantly by Ramadan fasting. Most of these metabolites were metabolites ratios (24), and the rest were three Glycolysis, three ketone bodies, nine Lipoprotein subclasses and one inflammation marker. This study suggests that Ramadan fasting is significantly associated with changes in the metabolic profile. However, the changes are assumed to be temporary, and the long-term effect of these changes is unknown.

Keywords: metabolic profile, Ramadan fasting, metabolites, intermittent fasting

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Authors: J. A. Sawicki, C. Ebrahimi

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The first geochemical, petrological, X-ray diffraction, Raman, Mössbauer, and oxygen isotopic analyses of very intriguing 13-kg Sooke #1 stone covered in 70% of its surface with black fusion crust, found in and recovered from Sooke Basin, near Juan de Fuca Strait, in British Columbia, were reported as poster #2775 at LPSC52 in March. Our further analyses reported in poster #6305 at 84AMMS in August and comparisons with the Mössbauer spectra of Martian meteorite MIL03346 and Martian rocks in Gusev Crater reported by Morris et al. suggest that Sooke #1 find could be a stony achondrite of Martian polymict breccia type ejected from early watery Mars. Here, the Raman spectra of a carbon-rich ~1-mm² fossil-like white area identified in this rock on a surface of polished cut have been examined in more detail. The low-intensity 532 nm and 633 nm beams of the InviaRenishaw microscope were used to avoid any destructive effects. The beam was focused through the microscope objective to a 2 m spot on a sample, and backscattered light collected through this objective was recorded with CCD detector. Raman spectra of dark areas outside fossil have shown bands of clinopyroxene at 320, 660, and 1020 cm-1 and small peaks of forsteritic olivine at 820-840 cm-1, in agreement with results of X-ray diffraction and Mössbauer analyses. Raman spectra of the white area showed the broad band D at ~1310 cm-1 consisting of main mode A1g at 1305 cm⁻¹, E2g mode at 1245 cm⁻¹, and E1g mode at 1355 cm⁻¹ due to stretching diamond-like sp3 bonds in diamond polytype lonsdaleite, as in Ovsyuk et al. study. The band near 1600 cm-1 mostly consists of D2 band at 1620 cm-1 and not of the narrower G band at 1583 cm⁻¹ due to E2g stretching in planar sp2 bonds that are fundamental building blocks of carbon allotropes graphite and graphene. In addition, the broad second-order Raman bands were observed with 532 nm beam at 2150, ~2340, ~2500, 2650, 2800, 2970, 3140, and ~3300 cm⁻¹ shifts. Second-order bands in diamond and other carbon structures are ascribed to the combinations of bands observed in the first-order region: here 2650 cm⁻¹ as 2D, 2970 cm⁻¹ as D+G, and 3140 cm⁻¹ as 2G ones. Nanodiamonds are abundant in the Universe, found in meteorites, interplanetary dust particles, comets, and carbon-rich stars. The diamonds in meteorites are presently intensely investigated using Raman spectroscopy. Such particles can be formed by CVD process and during major impact shocks at ~1000-2300 K and ~30-40 GPa. It cannot be excluded that the fossil discovered in Sooke #1 could be a remnant of an alien carbon organism that transformed under shock impact to nanodiamonds. We trust that for the benefit of research in astro-bio-geology of meteorites, asteroids, Martian rocks, and soil, this find deserves further, more thorough investigations. If possible, the Raman SHERLOCK spectrometer operating on the Perseverance Rover should also search for such objects in the Martian rocks.

Keywords: achondrite, nanodiamonds, lonsdaleite, raman spectra

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Authors: S. Palaniyappan, P. K. Chennam, M. Trautmann, H. Ahmad, T. Mehner, T. Lampke, G. Wagner

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In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al₂O₃)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al₂O₃ respectively. Raman spectroscopic analyses produced no characteristic bands of Al₂O₃, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Keywords: Al₂O₃ thin film, electrical insulation coating, PVD process, SiC fibre, single fibre tensile test

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Authors: Abdelrahman Zkria, Tsuyoshi Yoshitake

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Diamond is one of the most interesting semiconducting carbon materials owing to its unique physical and chemical properties, yet its application in electronic devices is limited due to the difficulty of realizing n-type conduction by nitrogen doping. In contrast Ultrananocrystalline diamond with diamond grains of about 3–5 nm in diameter have attracted much attention for device-oriented applications because they may enable the realization of n-type doping with nitrogen. In this study, nitrogen-doped Ultra-Nanocrystalline diamond films were prepared by coaxial arc plasma deposition (CAPD) method, the nitrogen content was estimated by X-ray photoemission spectroscopy (XPS). The electrical conductivity increased with increasing nitrogen contents. Heterojunction diodes with p-type Si were fabricated and evaluated based on current–voltage (I–V) and capacitance–voltage (C–V) characteristics measured in dark at room temperature.

Keywords: heterojunction diodes, hopping conduction mechanism, nitrogen-doping, ultra-nanocrystalline diamond

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Authors: Albert Mufundirwa, Satoru Yoshioka, K. Ogi, Takeharu Sugiyama, George F. Harrington, Bretislav Smid, Benjamin Cunning, Kazunari Sasaki, Akari Hayashi, Stephen M. Lyth

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Polymer electrolyte membrane fuel cells (PEMFCs) are electrochemical energy conversion devices used for portable, residential and vehicular applications due to their low emissions, high efficiency, and quick start-up characteristics. However, PEMFCs generally use expensive, Pt-based electrocatalysts as electrode catalysts. Due to the high cost and limited availability of platinum, research and development to either drastically reduce platinum loading, or replace platinum with alternative catalysts is of paramount importance. A combination of high surface area supports and nano-structured active sites is essential for effective operation of catalysts. We synthesize carbon foam supports by thermal decomposition of sodium ethoxide, using a template-free, gram scale, cheap, and scalable pyrolysis method. This carbon foam has a high surface area, highly porous, three-dimensional framework which is ideal for electrochemical applications. These carbon foams can have surface area larger than 2500 m²/g, and electron microscopy reveals that they have micron-scale cells, separated by few-layer graphene-like carbon walls. We applied this carbon foam as a platinum catalyst support, resulting in the improved electrochemical surface area and mass activity for the oxygen reduction reaction (ORR), compared to carbon black. Similarly, silver-decorated carbon foams showed higher activity and efficiency for electrochemical carbon dioxide conversion than silver-decorated carbon black. A promising alternative to Pt-catalysts for the ORR is iron-impregnated nitrogen-doped carbon catalysts (Fe-N-C). Doping carbon with nitrogen alters the chemical structure and modulates the electronic properties, allowing a degree of control over the catalytic properties. We have adapted our synthesis method to produce nitrogen-doped carbon foams with large surface area, using triethanolamine as a nitrogen feedstock, in a novel bottom-up protocol. These foams are then infiltrated with iron acetate (FeAc) and pyrolysed to form Fe-N-C foams. The resulting Fe-N-C foam catalysts have high initial activity (half-wave potential of 0.68 VRHE), comparable to that of commercially available Pt-free catalysts (e.g., NPC-2000, Pajarito Powder) in acid solution. In alkaline solution, the Fe-N-C carbon foam catalysts have a half-wave potential of 0.89 VRHE, which is higher than that of NPC-2000 by almost 10 mVRHE, and far out-performing platinum. However, the durability is still a problem at present. The lessons learned from X-ray absorption spectroscopy (XAS), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and electrochemical measurements will be used to carefully design Fe-N-C catalysts for higher performance PEMFCs.

Keywords: carbon-foam, polymer electrolyte membrane fuel cells, platinum, Pt-free, Fe-N-C, ORR

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Authors: S. Totong, P. Daorattanachai, N. Laosiripojana

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Lignin depolymerization into phenolic-based chemicals is an interesting process for utilizing and upgrading a benefit and value of lignin. In this study, the depolymerization reaction was performed to convert alkaline lignin into smaller molecule compounds. Fumed SiO₂ was used as a catalyst to improve catalytic activity in lignin decomposition. The important parameters in depolymerization process (i.e., reaction temperature, reaction time, etc.) were also investigated. In addition, gas chromatography with mass spectrometry (GC-MS), flame-ironized detector (GC-FID), and Fourier transform infrared spectroscopy (FT-IR) were used to analyze and characterize the lignin products. It was found that fumed SiO₂ catalyst led the good catalytic activity in lignin depolymerization. The main products from catalytic depolymerization were guaiacol, syringol, vanillin, and phenols. Additionally, metal supported on fumed SiO₂ such as Cu/SiO₂ and Ni/SiO₂ increased the catalyst activity in terms of phenolic products yield.

Keywords: alkaline lignin, catalytic, depolymerization, fumed SiO₂, phenolic-based chemicals

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

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

Keywords: biodeterioration, parchments, purple spots, ecological succession

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Authors: Muhammad Tariq, Muhammad Waseem, Muhammad Hidayat Rasool

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Isolation and characterization of chromium tolerant Staphylococcus aureus from industrial wastewater and their potential use to bioremediate environmental chromium. Objectives: Chromium with its great economic importance in industrial use is major metal pollutant of the environment. Chromium are used in different industries for various applications such as textile, dyeing and pigmentation, wood preservation, manufacturing pulp and paper, chrome plating, steel and tanning. The release of untreated chromium in industrial effluents causes serious threat to environment and human health, therefore, the current study designed to isolate chromium tolerant Staphylococcus aureus for removal of chromium prior to their final discharge into the environment due to its cost effective and beneficial advantage over physical and chemical methods. Methods: Wastewater samples were collected from discharge point of different industries. Heavy metal analysis by atomic absorption spectrophotometer and microbiological analysis such as total viable count, total coliform, fecal coliform and Escherichia coli were conducted. Staphylococcus aureus was identified through gram’s staining, biomeriux vitek 2 microbial identification system and 16S rRNA gene amplification by polymerase chain reaction. Optimum growth conditions with respect to temperature, pH, salt concentrations and effect of chromium on the growth of bacteria, resistance to other heavy metal ions, minimum inhibitory concentration and chromium uptake ability of Staphylococcus aureus strain K1 was determined by spectrophotometer. Antibiotic sensitivity pattern was also determined by disc diffusion method. Furthermore, chromium uptake ability was confirmed by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope equipped with Oxford Energy Dipersive X-ray (EDX) micro analysis system. Results: The results presented that optimum temperature was 35ᵒC, pH was 8.0 and salt concentration was 0.5% for growth of Staphylococcus aureus K1. The maximum uptake ability of chromium by bacteria was 20mM than other heavy metal ions. The antibiotic sensitivity pattern revealed that Staphylococcus aureus was vancomycin and methicillin sensitive. Non hemolytic activity on blood agar and negative coagulase reaction showed that it was non-pathogenic. Furthermore, the growth of bacteria decreases in the presence of chromium and maximum chromium uptake by bacteria observed at optimum growth conditions. Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and Energy dispersive X-ray (EDX) analysis confirmed the presence of chromium uptake by Staphylococcus aureus K1. Conclusion: The study revealed that Staphylococcus aureus K1 have the potential to bio-remediate chromium toxicity from wastewater. Gradually, this biological treatment becomes more important due to its advantage over physical and chemical methods to protect environment and human health.

Keywords: wastewater, staphylococcus, chromium, bioremediation

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Authors: Dibyendu Adak, Saroj Mandal

Abstract:

The fly ash based geopolymer concrete generally requires heat activation after casting, which has been considered as an important limitation for its practical application. Such limitation can be overcome by a modification in the process at the time of mixing of ingredients (fly and activator fluid) for geopolymer concrete so that curing can be made at ambient temperature. This process modified geopolymer concrete shows an appreciable improvement in structural performance compared to conventional heat cured geopolymer concrete and control cement concrete. The improved durability performance based on water absorption, sulphate test, and RCPT is also noted. The microstructural properties analyzed through Field Emission Scanning Electron Microscope (FESEM) with Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD) techniques show the better interaction of fly ash and activator solution at early ages for the process modified geopolymer concrete. This accelerates the transformation of the amorphous phase of fly ash to the crystalline phase.

Keywords: fly ash, geopolymer concrete, process modification, structural properties, durability, micro-structures

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Authors: O. Çomaklı, M. Yazıcı, T. Yetim, A. F. Yetim, A. Çelik

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In this work, TiO₂ films were deposited on Cp-Ti substrates by thermal oxidation, DC plasma oxidation, and by the sol-gel method. Microstructures of uncoated and TiO₂ film coated samples were examined by X-ray diffraction and SEM. Thin oxide film consisting of anatase (A) and rutile (R) TiO₂ structures was observed on the surface of CP-Ti by under three different treatments. Also, the more intense anatase and rutile peaks appeared at samples plasma oxidized at 700˚C. The thicknesses of films were about 1.8 μm at the TiO₂ film coated samples by sol-gel and about 2.7 μm at thermal oxidated samples, while it was measured as 3.9 μm at the plasma oxidated samples. Electrochemical corrosion behaviour of uncoated and coated specimens was mainly carried out by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) in simulated body fluid (SBF) solution. Results showed that at the plasma oxidated samples exhibited a better resistance property to corrosion than that of other treatments.

Keywords: TiO₂, CP-Ti, corrosion properties, thermal oxidation, plasma oxidation, sol-gel

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Authors: Muhammad Akbar Hussain, Muhammad Mehdi Hussain, Waqar Haider

Abstract:

There are tens of thousands of undetected and uncatalogued pieces of space debris in the Low Earth Orbit (LEO). They are not only difficult to be detected and tracked, their sheer number puts active satellites and humans in orbit around Earth into danger. With the entry of more governments and private companies into harnessing the Earth’s orbit for communication, research and military purposes, there is an ever-increasing need for not only the detection and cataloguing of these pieces of space debris, it is time to take measures to take them out and clean up the space around Earth. Current optical and radar-based Space Situational Awareness initiatives are useful mostly in detecting and cataloguing larger pieces of debris mainly for avoidance measures. Smaller than 10 cm pieces are in a relatively dark zone, yet these are deadly and capable of destroying satellites and human missions. A network of mobile observatories, connected to each other in real time and working in unison as a single instrument, may be able to detect small pieces of debris and achieve effective triangulation to help create a comprehensive database of their trajectories and parameters to the highest level of precision. This data may enable ground-based laser systems to help deorbit individual debris. Such a network of observatories can join current efforts in detection and removal of space debris in Earth’s orbit.

Keywords: space debris, low earth orbit, mobile observatories, triangulation, seamless operability

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

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

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

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Authors: Esther Lorrayne M. Pereira, Adriana S. M. Batista, Fabíola A. S. Ribeiro, Adelina P. Santos, Luiz O. Faria

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In this work we have prepared nanocomposites made by mixing Poli (vinilidene fluoride) (PVDF), zirconium oxide (ZrO₂) and multi–walled carbon nanotubes (MWCNTs) aiming to find dosimetric properties for applications in high dose dosimetry. The samples were irradiated with a Co-60 source at constant dose rate (16.7 kGy/h), with doses ranging from 100 to 2750 kGy. The UV-Vis and FTIR spectrophotometry have been used to monitor the appearing of C=C conjugated bonds and radio-oxidation of carbon (C=O). FTIR spectrometry has that the absorbance intensities at 1715 cm⁻¹ and 1730 cm⁻¹ can be used for high dosimetry purposes for gamma doses ranging from 500 to 2750 kGy. In this range, it is possible to observe a linear relationship between Abs & Dose. Fading of signal was evaluated for one month and reproducibility in 2000 kGy dose. Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) was used for evaluated the dispersion ZrO₂ and MWCNT in the matrix of the PVDF.

Keywords: polymer, composite, high dose dosimetry, PVDF/ZrO₂/MWCNT

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Authors: Burcu Kiren, Alattin CAkan, Nezihe Ayas

Abstract:

Hydrogen will be arguably the best fuel in the future as it is the most abundant element in the universe. Hydrogen, as a fuel, is notably environmentally benign, sustainable and has high energy content compared to other sources of energy. It can be generated from both conventional and renewable sources. The hydrolysis reaction of metal hydrides provides an option for hydrogen production in the presence of a catalyst. In this study, Ni/dolomite catalyst was synthesized by the wet impregnation method for hydrogen production by hydrolysis reaction of sodium borohydride (NaBH4). Besides, the synthesized catalysts characterizations were examined by means of thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer –Emmett – Teller (BET) and scanning electron microscopy (SEM). The influence of reaction temperature (25-75 °C), reaction time (15-60 min.), amount of catalyst (50-250 mg) and active metal loading ratio (20,30,40 wt.%) were investigated. The catalyst prepared with 30 wt.% Ni was noted as the most suitable catalyst, achieving of 35.18% H₂ and hydrogen production rate of 19.23 mL/gcat.min at 25 °C at reaction conditions of 5 mL of 0.25 M NaOH and 100 mg NaBH₄, 100 mg Ni/dolomite.

Keywords: sodium borohydride, hydrolysis, catalyst, Ni/dolomite, hydrogen

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Authors: Ayodele Odularu, Peter Ajibade, Albert Bolhuis

Abstract:

This study aimed at assessing the antibacterial activities of four zinc (II) complexes. Zinc (II) complexes of nitrogen, oxygen and sulfur coordination modes were synthesized using direct substitution reaction. The characterization techniques involved physicochemical properties (molar conductivity) and spectroscopic techniques. The molar conductivity gave the non-electrolytic nature of zinc (II) complexes. The spectral studies of zinc (II) complexes were done using electronic spectra (UV-Vis) and Fourier Transform Infra-red Spectroscopy (FT-IR). Spectral data from the spectroscopic studies confirmed the coordination of the mixed ligands with zinc (II) ion. The antibacterial activities of zinc(II) complexes of were all in supportive of Overtone’s concept and Tweedy’s theory of chelation for bacterial strains of S. aureus MRSA252 and E coli MC4100 because the zones of inhibition were greater than the corresponding ligands. In summary, all zinc (II) complexes of ZEPY, ZE1PH, ZE1PY and ZE135PY all have potentials for antibacterial activities.

Keywords: antibacterial activities, spectral studies, syntheses, zinc(II) complexes

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Authors: Mei Hong, Wei Liu, Xuemin Dai, Yanxiong Pan, Xiangling Ji

Abstract:

Polyamic acid (PAA) is the precursor of polyimide (PI) prepared by a two-step method, its molecular weight and molecular weight distribution not only play an important role during the preparation and processing, but also influence the final performance of PI. However, precise characterization on molecular weight of PAA is still a challenge because of the existence of very complicated interactions in the solution system, including the electrostatic interaction, hydrogen bond interaction, dipole-dipole interaction, etc. Thus, it is necessary to establisha suitable strategy which can completely suppress these complex effects and get reasonable data on molecular weight. Herein, the gel permeation chromatography (GPC) coupled with differential refractive index (RI) and multi-angle laser light scattering (MALLS) detectors were applied to measure the molecular weight of (6FDA-DMB) PAA using different mobile phases, LiBr/DMF, LiBr/H3PO4/THF/DMF, LiBr/HAc/THF/DMF, and LiBr/HAc/DMF, respectively. It was found that combination of LiBr with HAc can shield the above-mentioned complex interactions and is more conducive to the separation of PAA than only addition of LiBr in DMF. LiBr/HAc/DMF was employed for the first time as a mild mobile phase to effectively separate PAA and determine its molecular weight. After a series of conditional experiments, 0.02M LiBr/0.2M HAc/DMF was fixed as an optimized mobile phase to measure the relative and absolute molecular weights of (6FDA-DMB) PAA prepared, and the obtained Mw from GPC-MALLS and GPC-RI were 35,300 g/mol and 125,000 g/mol, respectively. Particularly, such a mobile phase is also applicable to other PAA samples with different structures, and the final results on molecular weight are also reproducible.

Keywords: Polyamic acids, Polyelectrolyte effects, Gel permeation chromatography, Mobile phase, Molecular weight

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Authors: Manel Hannachi, Mustapha Nechiche, Said Azem

Abstract:

This study focuses on biodegradable materials made from Poly-lactic acid (PLA) and vegetal reinforcements. Three materials are developed from PLA, as a matrix, and : (i) olive kernels (OK); (ii) alfa (α) short fibers and (iii) OK+ α mixture, as reinforcements. After processing of PLA pellets and olive kernels in powder and alfa stems in short fibers, three mixtures, namely PLA-OK, PLA-α, and PLA-OK-α are prepared and homogenized in Turbula®. These mixtures are then compacted at 180°C under 10 MPa during 15 mn. Scanning Electron Microscopy (SEM) examinations show that PLA matrix adheres at surface of all reinforcements and the dispersion of these ones in matrix is good. X-ray diffraction (XRD) analyses highlight an increase of PLA inter-reticular distances, especially for the PLA-OK case. These results are explained by the dissociation of some molecules derived from reinforcements followed by diffusion of the released atoms in the structure of PLA. This is consistent with Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) analysis results.

Keywords: alfa short fibers, biodegradable composite, olive kernels, poly-lactic acid

Procedia PDF Downloads 147

Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

Abstract:

This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, ¹H and ¹³C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]⁺ peaks at m/z 312, which are in agreement to the calculated molecular weight. For ¹H NMR spectra, the presence of OCH₃, C=S-NH and C=O-NH protons were observed within range of δ_H 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. ¹³C NMR spectra in all compounds displayed the presence of OCH₃, C=O-NH, C=O-OH and C=S carbon resonances within range of δ_C 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm^-1, 2976-3302 cm^-1, 1720-1768 cm^-1, 1655-1672 cm^-1, 1519-1525 cm^-1 and 754-763 cm^-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial

Procedia PDF Downloads 332