Search results for: (FTIR) spectroscopy

Authors: Dilip Saikia, Suparna Bhattacharjee, Nirab Adhikary

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In this piece of work, we have presented the synthesis and characterization of CdTe/ZnS core/shell (CS) quantum dots (QD). CS QDs are used as a fluorescence probe to design a simple cost-effective and ultrasensitive sensor for the detection of toxic Hg(II) in an aqueous medium. Mercaptosuccinic acid (MSA) has been used as a capping agent for the synthesis CdTe/ZnS CS QD. Photoluminescence quenching mechanism has been used in the detection experiment of Hg(II). The designed sensing technique shows a remarkably low detection limit of about 1 picomolar (pM). Here, the CS QDs are synthesized by a simple one-pot aqueous method. The synthesized CS QDs are characterized by using advanced diagnostics tools such as UV-vis, Photoluminescence, XRD, FTIR, TEM and Zeta potential analysis. The interaction between CS QDs and the Hg(II) ions results in the quenching of photoluminescence (PL) intensity of QDs, via the mechanism of excited state electron transfer. The proposed mechanism is explained using cyclic voltammetry and zeta potential analysis. The designed sensor is found to be highly selective towards Hg (II) ions. The analysis of the real samples such as drinking water and tap water has been carried out and the CS QDs show remarkably good results. Using this simple sensing method we have designed a prototype low-cost electronic device for the detection of Hg(II) in an aqueous medium. The findings of the experimental results of the designed sensor is crosschecked by using AAS analysis.

Keywords: photoluminescence, quantum dots, quenching, sensor

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Authors: Illyas Isa, Mohamad Idris Saidin, Mustaffa Ahmad, Norhayati Hashim

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A highly selective and sensitive electrode for determination of trace amounts of Cu (II) using square wave anodic stripping voltammetry (SWASV) was proposed. The electrode was made of the paste of multiwall carbon nanotubes (MWCNT) and 2,6–diacetylpyridine-di-(1R)–(-)–fenchone diazine tetracarbonylmolybdenum(0) at 100:5 (w/w). Under optimal conditions the electrode showed a linear relationship with concentration in the range of 1.0 × 10–10 to 1.0 × 10– 6 M Cu (II) and limit of detection 8.0 × 10–11 M Cu (II). The relative standard deviation (n = 5) of response to 1.0 × 10–6 M Cu(II) was 0.036. The interferences of cations such as Ni(II), Mg(II), Cd(II), Co(II), Hg(II), and Zn(II) (in 10 and 100-folds concentration) are negligible except from Pb (II). Electrochemical impedance spectroscopy (EIS) showed that the charge transfer at the electrode-solution interface was favorable. Result of analysis of Cu(II) in several water samples agreed well with those obtained by inductively coupled plasma-optical emission spectrometry (ICP-OES). The proposed electrode was then recommended as an alternative to spectroscopic technique in analyzing Cu (II).

Keywords: chemically modified electrode, Cu(II), Square wave anodic stripping voltammetry, tetracarbonylmolybdenum(0)

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Authors: Iordana Neamtu, Aurica P. Chiriac, Loredana E. Nita, Mihai Asandulesa, Elena Butnaru, Nita Tudorachi, Alina Diaconu

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In the last decade, the attention of many researchers is focused on the synthesis of innovative “intelligent” copolymer structures with great potential for different uses. This considerable scientific interest is stimulated by possibility of the significant improvements in physical, mechanical, thermal and other important specific properties of these materials. Functionalization of polymer in synthesis by designing a suitable composition with the desired properties and applications is recognized as a valuable tool. In this work is presented a comparative study of the properties of the new copolymers poly(maleic anhydride maleic-co-3,9-divinyl-2,4,8,10-tetraoxaspiro[5.5]undecane) and poly(itaconic-anhydride-co-3,9-divinyl-2,4,8,10-tetraoxaspiro[5.5]undecane) obtained by radical polymerization in dioxane, using 2,2′-azobis(2-methylpropionitrile) as free-radical initiator. The comonomers are able for generating special effects as for example network formation, biodegradability and biocompatibility, gel formation capacity, binding properties, amphiphilicity, good oxidative and thermal stability, good film formers, and temperature and pH sensitivity. Maleic anhydride (MA) and also the isostructural analog itaconic anhydride (ITA) as polyfunctional monomers are widely used in the synthesis of reactive macromolecules with linear, hyperbranched and self & assembled structures to prepare high performance engineering, bioengineering and nano engineering materials. The incorporation of spiroacetal groups in polymer structures improves the solubility and the adhesive properties, induce good oxidative and thermal stability, are formers of good fiber or films with good flexibility and tensile strength. Also, the spiroacetal rings induce interactions on ether oxygen such as hydrogen bonds or coordinate bonds with other functional groups determining bulkiness and stiffness. The synthesized copolymers are analyzed by DSC, oscillatory and rotational rheological measurements and dielectric spectroscopy with the aim of underlying the heating behavior, solution viscosity as a function of shear rate and temperature and to investigate the relaxation processes and the motion of functional groups present in side chain around the main chain or bonds of the side chain. Acknowledgments This work was financially supported by the grant of the Romanian National Authority for Scientific Research, CNCS-UEFISCDI, project number PN-II-132/2014 “Magnetic biomimetic supports as alternative strategy for bone tissue engineering and repair’’ (MAGBIOTISS).

Keywords: Poly(maleic anhydride-co-3, 9-divinyl-2, 4, 8, 10-tetraoxaspiro (5.5)undecane); Poly(itaconic anhydride-co-3, 9-divinyl-2, 4, 8, 10-tetraoxaspiro (5.5)undecane); DSC; oscillatory and rotational rheological analysis; dielectric spectroscopy

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Authors: Badis Kahouadji, Lakhdar Guerbous, Lyes Lamiri

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For many years, the luminescent materials were investigated principally in the infrared and visible areas, because the ultraviolet (UV) and especially in vacuum Ultraviolet (VUV) are technically more difficult to explore, especially absence of applications requiring of materials suitable to short wavelengths.Recent necessary, related to the development of certain technologies, encouraged research in these spectra domains. It is in this context that the 4Fn-4Fn-1 5d transitions of rare earth in insulating materials, lying in the UV and VUV, are the aim of large number of studies. These studies relate in particular to search for new scintillator materials used for spectroscopy and X-ray, ɤ, as well as medical imaging. The 4Fn- 4Fn-15d transitions of the rare earth dependent to the host-matrix, several matrices ions were used to study these transitions, in this work we are suggeting to study on a very specific class of inorganic scintillators that are orthophosphate doped with rare earth ions, this study focused on the Pr3+ concentration on the structural and optical properties of Pr3+ doped YPO4 (yttriumorthophosphate) with powder form prepared by the Sol Gel method.

Keywords: rare earth, scintillator, YPO4:Pr3+ nanophosphors, sol gel, 4Fn-4Fn-15d transitions

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Authors: H. Mokaddem, D. Miroud, N. Azouaou, F. Si-Ahmed, Z. Sadaoui

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The synthesis and characterization of activated carbon from local lignocellulosic precursor (Algerian alfa) was carried out for the removal of cationic dyes from aqueous solutions. The effect of the production variables such as impregnation chemical agents, impregnation ratio, activation temperature and activation time were investigated. Carbon obtained using the optimum conditions (CaCl2/ 1:1/ 500°C/2H) was characterized by various analytical techniques scanning electron microscopy (SEM), infrared spectroscopic analysis (FTIR) and zero-point-of-charge (pHpzc). Adsorption tests of methylene blue on the optimal activated carbon were conducted. The effects of contact time, amount of adsorbent, initial dye concentration and pH were studied. The adsorption equilibrium examined using Langmuir, Freundlich, Temkin and Redlich–Peterson models reveals that the Langmuir model is most appropriate to describe the adsorption process. The kinetics of MB sorption onto activated carbon follows the pseudo-second order rate expression. The examination of the thermodynamic analysis indicates that the adsorption process is spontaneous (ΔG ° < 0) and endothermic (ΔH ° > 0), the positive value of the standard entropy shows the affinity between the activated carbon and the dye. The present study showed that the produced optimal activated carbon prepared from Algerian alfa is an effective low-cost adsorbent and can be employed as alternative to commercial activated carbon for removal of MB dye from aqueous solution.

Keywords: activated carbon, adsorption, cationic dyes, Algerian alfa

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Authors: Ruma Rano, Firoza Sultana, Bishal Bhuyan, Nurul Alam Mazumder

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Fly ash collected from Cachar Paper Mill, Assam, India has been thoroughly characterized in respect of its physico-chemical, morphological and mineralogical features were concerned by using density, LOI, FTIR, XRD, SEM-EDS etc. The results reveal that there is a striking difference in the features and properties of the coarser and finer fractions .The high carbon ash consists of large unburnt carbon (chars), irregular carbonaceous particles in the coarser fraction, which appear to be porous and may be used as domestic fuel. The percentage of char albeit the carbon content decreases with decrease in size of particles. The various fractions essentially contain quartz and mullite as the main mineral phases. For suggesting the potential utilization channels, number of experiments were performed correlating the total characteristic features. Water holding capacities of different size classified fractions were determined, the coarser fractions have unexpectedly higher water holding capacities than the finer ones. An attempt has been made to correlate the results obtained with potential use in agriculture. Another potential application of coarser particles is used as adsorbent for effluents containing waste organic materials. Thus thorough characterization leads to not only a definite direction about the uses of the value added components but also gives useful information regarding the prevailing combustion process.

Keywords: chars, porous, water holding capacity, combustion process

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Authors: J. Chandrasekhar Rao, B. G. Naidu, G. J. Naga Raju, P. Sarita

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Particle Induced X-ray Emission (PIXE) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) techniques have been employed in this work to determine the elements present in the root of Cyperus rotundus medicinal plant used in the treatment of rheumatoid arthritis. The elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, and Sr were commonly identified and quantified by both PIXE and ICP-MS whereas the elements Li, Be, Al, As, Se, Ag, Cd, Ba, Tl, Pb and U were determined by ICP-MS and Cl, K, Ca, Ti and Br were determined by PIXE. The regional variation of elemental content has also been studied by analyzing the same plant collected from different geographical locations. Information on the elemental content of the medicinal plant would be helpful in correlating its ability in the treatment of rheumatoid arthritis and also in deciding the dosage of this herbal medicine from the metal toxicity point of view. Principal component analysis and cluster analysis were also applied to the data matrix to understand the correlation among the elements.

Keywords: PIXE, CP-MS, elements, Cyperus rotundus, rheumatoid arthritis

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Authors: Atef Youssef, Marwa Mostafa Moharam

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The effects of poly pyrrole (PP) addition on LiFePO4 have been studied by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and galvanostatic measurements. PP was prepared with LiFePO₄ in different ways, such as chemically dispersion, insinuation polymerization, and electrochemically polymerization. The EIS results showed that the charge transfer resistance (Rct) of LiFePO₄ was decreased by adding 10% PP polymerized in a situation to 153 vs. 1660  for bare LiFePO₄. The CV curves show that 10% PP added LiFePO₄ had higher electrochemical reactivity for lithium insertion and extraction than the un-doped material. The mean redox potential is E1/2 = 3.45 V vs. Li+/Li. The first discharge curve of the 10% poly pyrrole doped LiFePO₄ showed a mainly flat voltage plateau over the 3.45–3.5 V range, indicating the lithium extraction and insertion reactions between LiFePO₄ and FePO₄. A specific discharge capacity of cells prepared from in-situ 10% PP added LiFePO4to was about 210 vs. 65 mAhg-1 for bare LiFePO₄.

Keywords: liFePO₄, poly pyrrole addition, positive electrode, lithium battery

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Authors: Aigin Bashti

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Preparation of multicomponent reactions (MCRs) via a simple one-pot strategy is considered a novel procedure which has attracted a lot of interest from organic and medicinal chemists. Due to the great importance of phthalazide triones, it was decided to introduce a novel and cost-effective green procedure for the preparation of these derivatives. In this methodology, an efficient 4,4ʹ-Bipyridinium Dichloride Ordered Mesoporous Silica functionalized catalyst (BP-SBA-15) was utilized. The catalyst was characterized by X-ray diffraction analysis (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FT-IR) analysis. In conclusion, it should be mentioned that this methodology has some advantages, including short reaction time, high yield of the products, recyclable catalyst, green procedure, and facile work-up procedure. The catalyst was successfully utilized for the one-pot preparation of various phthalazinetrione derivatives.

Keywords: dimedone, green procedure, multicomponent reactions, phthalhydrazide

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Authors: T. V. Dinh, I. Y. Choi, J. W. Ahn, Y. H. Oh, G. Bo, J. Y. Lee, J. C. Kim

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A Non-Dispersive Infrared (NDIR) multi-gas analyzer has been developed to monitor the emission of carbon monoxide (CO) and sulfur dioxide (SO2) from various industries. The NDIR technique for gas measurement is based on the wavelength absorption in the infrared spectrum as a way to detect particular gasses. NDIR analyzers have popularly applied in the Tele-Monitoring System (TMS). The advantage of the NDIR analyzer is low energy consumption and cost compared with other spectroscopy methods. However, zero/span drift and interference are its urgent issues to be solved. Multi-pathway technique based on optical White cell was employed to improve the sensitivity of the analyzer in this work. A pyroelectric detector was used to detect the Infrared radiation. The analytical range of the analyzer was 0 ~ 200 ppm. The instrument response time was < 2 min. The detection limits of CO and SO2 were < 4 ppm and < 6 ppm, respectively. The zero and span drift of 24 h was less than 3%. The linearity of the analyzer was less than 2.5% of reference values. The precision and accuracy of both CO and SO2 channels were < 2.5% of relative standard deviation. In general, the analyzer performed well. However, the detection limit and 24h drift should be improved to be a more competitive instrument.

Keywords: analyzer, CEMS, monitoring, NDIR, TMS

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Authors: César Oliveira, Ana M. S. Bettencourt, Luciano Vilas Boas, Luís Gonçalves, Carlo Bottaini

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Funerary megalithic monuments are probably under the most remarkable remains of the Neolithic period of western Europe. Some monuments are well known for their paintings, sometimes associated with engraved motifs, giving the funerary crypts a character of great symbolic value. The engraved and painted motifs, the colors used in the paintings, and the offerings associated with the deposited corpses are archaeological data that, being part of the funeral rites, also reveal the ideological world of these communities and their way of interacting with the world. In this sense, the choice of colors to be used in the paintings, the pigments collected, and the proceeds for making the paints would also be significant performances. The present study will focus on the characterization of painted art from megalithic monuments located in different areas of North-Western Portugal (coastal and inland). The colorant composition of megalithic barrows decorated with rock art motifs was studied using a multi-analytical approach (XRD, SEM-EDS, FTIR, and GC-MS), allowing the characterization of the painting techniques, pigments, and the organic compounds used as binders. Some analyses revealed that the pigments used for painting were produced using a collection of mined or quarried organic and inorganic substances. The results will be analyzed from the perspective of contingencies and regularity among the different case studies in order to interpret more or less standardized behaviors.

Keywords: funerary megalithic monuments, painting motifs, archaeometrical studies, Northwest Iberia, behaviors

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Authors: Samira Ghizellaoui, Manel Boumagoura, Rayane Menzri

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The ground water Hamma rich in calcium and bicarbonate likely to deposit the tartar and subsequently lead to the obstruction of the pipes and the seizing of the stopping devices in addition to the financial losses resulting there from. It is therefore necessary to optimise an antiscaling treatment in order to avoid the risk of formation of tartar deposits in the various installations and to protect the equipment in contact with this water. MgCl2 is the chemical inhibitor which was tested. To optimise the effective concentration of this product, we used two electrochemical methods (chronoamperometry and impedancemetry) to identify the best method for optimizing antiscaling treatment. IR, RX, Raman spectroscopy and SEM indicate that the raw waters of Hamma give precipitates in the form of calcite (the most stable form), with the presence of a small amount of magnesian calcite and aragonite. In the presence of the inhibitor (MgCl2), calcium carbonate changes morphology to other forms that do not exist in the deposit obtained from the raw water (vaterite and calcium carbonate monohydrate).

Keywords: calcium carbonate, MgCl2, chronoamperometry, Impedancemetry

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Authors: Laura Kocsor, Laszlo Peter, Laszlo Kovacs, Zsolt Kis

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The aim of our research is to prepare rare-earth-doped lithium niobate (LiNbO3) nanocrystals, having only a few dopant ions in the focal point of an exciting laser beam. These samples will be used to achieve individual addressing of the dopant ions by light beams in a confocal microscope setup. One method for the preparation of nanocrystalline materials is to reduce the particle size by mechanical grinding. High-energy ball-milling was used in several works to produce nano lithium niobate. Previously, it was reported that dry high-energy ball-milling of lithium niobate in a shaker mill results in the partial reduction of the material, which leads to a balanced formation of bipolarons and polarons yielding gray color together with oxygen release and Li2O segregation on the open surfaces. In the present work we focus on preparing LiNbO3 nanocrystals by high-energy ball-milling using a Fritsch Pulverisette 7 planetary mill. Every ball-milling process was carried out in zirconia vial with zirconia balls of different sizes (from 3 mm to 0.1 mm), wet grinding with water, and the grinding time being less than an hour. Gradually decreasing the ball size to 0.1 mm, an average particle size of about 10 nm could be obtained determined by dynamic light scattering and verified by scanning electron microscopy. High-energy ball-milling resulted in sample darkening evidenced by optical absorption spectroscopy measurements indicating that the material underwent partial reduction. The unwanted lithium oxide loss decreases the Li/Nb ratio in the crystal, strongly influencing the spectroscopic properties of lithium niobate. Zirconia contamination was found in ground samples proved by energy-dispersive X-ray spectroscopy measurements; however, it cannot be explained based on the hardness properties of the materials involved in the ball-milling process. It can be understood taking into account the presence of lithium hydroxide formed the segregated lithium oxide and water during the ball-milling process, through chemically induced abrasion. The quantity of the segregated Li2O was measured by coulometric titration. During the wet milling process in the planetary mill, it was found that the lithium oxide loss increases linearly in the early phase of the milling process, then a saturation of the Li2O loss can be seen. This change goes along with the disappearance of the relatively large particles until a relatively narrow size distribution is achieved in accord with the dynamic light scattering measurements. With the 3 mm ball size and 1100 rpm rotation rate, the mean particle size achieved is 100 nm, and the total Li2O loss is about 1.2 wt.% of the original LiNbO3. Further investigations have been done to minimize the Li2O segregation during the ball-milling process. Since the Li2O loss was observed to increase with the growing total surface of the particles, the influence of ball-milling parameters on its quantity has also been studied.

Keywords: high-energy ball-milling, lithium niobate, mechanochemical reaction, nanocrystals

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Authors: Buno Henriques, Rafaela Santos, Júlio Matias de Souza, Filipe Silva, Rubens Nascimento, Márcio Fredel

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Dental porcelain composites reinforced and toughened by 20 wt.% tetragonal zirconia (3Y-TZP) were processed by hot pressing at 1000°C. Two types of particles were tested: yttria-stabilized zirconia (ZrO2–3%Y2O3) agglomerates and pre-sintered yttria-stabilized zirconia (ZrO2–3%Y2O3) particles. The composites as well as the reinforcing particles were analyzed by the means of optical and Scanning Electron Microscopy (SEM), Energy Dispersion Spectroscopy (EDS) and X-Ray Diffraction (XRD). The mechanical properties were obtained by the transverse rupture strength test, Vickers indentations and fracture toughness. Wear tests were also performed on the composites and monolithic porcelain. The best mechanical and wear results were displayed by the porcelain reinforced with the pre-sintered ZrO2–3%Y2O3 particles.

Keywords: dental restoration, zirconia, porcelain, composites, strengthening, toughening, wear

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are generally used for designing the core components of nuclear reactors due to their good mechanical and tribological properties. Some core components are subjected to flow-induced vibrations resulting in wear of these components due to their interaction with one another. To simulate these conditions, low amplitude reciprocating wear tests are conducted at room temperature and high temperature (260 degrees Celsius) between Zr-2.5Nb alloy and SS-410. The tests are conducted at a frequency range of 5 Hz to 25 Hz and an amplitude range of 200 µm to 600 µm. Friction and wear responses were recorded and correlated with the change in parameters. Worn surfaces are analysed using scanning electron microscopy (SEM) and optical profilometer. Elemental changes on the worn surfaces were determined using energy dispersive spectroscopy (EDS). The coefficient of friction (COF) increases with increasing temperature and decreases with increasing frequency. Adhesive wear is found to be the dominant wear mechanism which increases at high temperature.

Keywords: nuclear reactor, Zr-2.5Nb, SS-410, friction and wear

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Authors: Yasaman Tabari-Saadi, Kaiwen Sun, Jialiang Huang, Martin Green, Xiaojing Hao

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Optical and electrical properties of p-type AgBiS₂ absorber material have been improved by copper doping on silver sites. X-Ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analysis suggest that complete solid solutions of Ag₁₋ₓCuₓBiS₂ thin film have been formed. The carrier concentration of pure AgBiS₂ thin film deposited by the chemical process is 4.5*E+14 cm⁻³, and copper doping leads to the improved carrier concentration despite the semiconductor AgBiS₂ remains p-type semiconductor. Copper doping directly changed the absorption coefficient and increased the optical band gap (~1.5eV), which makes it a promising absorber for thin-film solar cell applications.

Keywords: copper doped, AgBiS₂, thin-film solar cell, carrier concentration, p-type semiconductor

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Authors: Soner Cubuk, Mirgul Kosif, M. Vezir Kahraman, Ece Kok Yetimoglu

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Boron is an essential trace element for the completion of the life circle for organisms. Suitable methods for the determination of boron have been proposed, including acid - base titrimetric, inductively coupled plasma emission spectroscopy flame atomic absorption and spectrophotometric. However, the above methods have some disadvantages such as long analysis times, requirement of corrosive media such as concentrated sulphuric acid and multi-step sample preparation requirements and time-consuming procedures. In this study, a selective and reusable fluorescent sensor for boron based on glycosyloxyethyl methacrylate was prepared by photopolymerization. The response characteristics such as response time, pH, linear range, limit of detection were systematically investigated. The excitation/emission maxima of the membrane were at 378/423 nm, respectively. The approximate response time was measured as 50 sec. In addition, sensor had a very low limit of detection which was 0.3 ppb. The sensor was successfully used for the determination of boron in water samples with satisfactory results.

Keywords: boron, fluorescence, photopolymerization, polymeric sensor

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Authors: Souha Bouagila, Soufiene Ilahi, Noureddine Yacoubi

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We have used Photothermal deflection spectroscopy PTD to investigate the impact of thermal annealing on electronics properties of GaInAsSb/GaSb.GaInAsSb used as an active layer for Vertical Cavity Surface Emitting laser (VCSEL). We have remarked that surface recombination velocity (SRV) from 7963 m / s (± 6.3%) to 1450 m / s (± 3.6) for as grown to sample annealed for 60 min. Accordingly, Force Microscopy images analyses agree well with the measure of surface recombination velocity. We have found that Root-Mean-Square Roughness (RMS) decreases as respect of annealing time. In addition, we have that the diffusion length and minority carrier mobility have been enhanced according to annealing time. However, due to annealing effects, the interface recombination velocity (IRV) is increased from 1196 m / s (± 5) to 6000 m/s (5%) for GaInAsSb in respect of annealed times.

Keywords: nonradiative lifetime, mobility of minority carrier, diffusion length, Surface and interface recombination velocity

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Authors: Eduardo Padilla, Luis Daniel Rodriguez, Ivan Sanchez, Angelica Sofia Go

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The synthesis and application of metallic nanoparticles have increased in recent years. Biological methods go beyond the chemical and physical synthesis that is expensive and not friendly to the environment. Therefore, in this study, silver nanoparticles were synthesized biologically in an environmentally friendly way by Handroanthus chrysanthus flower aqueous extract (AgNPs) that contains phytochemicals capable of reducing silver nitrate. AgNPs were characterized visually by UV-visible spectroscopy and TEM. The antimicrobial activity of the AgNPs was tested by determining the minimum inhibitory concentration (MIC), and minimal bactericidal concentration (MBC) in Escherichia coli and Staphylococcus aureus strains AgNPs showed potent antimicrobial activity against gram-negative and gram-positive bacteria. MIC and MBC values were as low as 41.6, and 83.2 ug/mL using AgNPs biosynthesized by H. chrysanthus flower extract. This nanoparticle could be the basis for the formulation of disinfectants for use in the food and pharmaceutical industry.

Keywords: antimicrobial, silver nanoparticles, flower extract, Handroanthus

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Authors: Najme Lari, Shahrokh Ahangarani, Ali Shanaghi

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Sol-gel technology is a promising manufacturing method to produce anti reflective silica thin films for solar energy applications. So to improve the properties of the films, controlling parameter of the sol - gel method is very important. In this study, soaking treatment effect on optical properties of silica anti reflective thin films was investigated. UV-Visible Spectroscopy, Fourier-Transformed Infrared Spectrophotometer and Field Emission Scanning Electron Microscopy was used for the characterization of silica thin films. Results showed that all nanoporous silica layers cause to considerable reduction of light reflections compared with uncoated glasses. With single layer deposition, the amount of reduction depends on the dipping time of coating and has an optimal time. Also, it was found that solar transmittance increased from 91.5% for the bare slide up to 97.5% for the best made sample corresponding to two deposition cycles.

Keywords: sol–gel, silica thin films, anti reflective coatings, optical properties, soaking treatment

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Authors: Amrei Voelkner, Nils Peters, Thomas Mannheim

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The worldwide exponential growth of the population and the simultaneous increasing food production requires the strategic realization of sustainable and improved cultivation systems to ensure the fertility of arable land and to guarantee the food supply for the whole world. To fulfill this target, large quantities of fertilizers have to be applied to the field, but the long-term environmental impacts remain uncertain. Thus, a combined system would be necessary to increase the nutrient availability for plants while reducing nutrient losses (e.g. NO3- by leaching) to the environment. To enhance the nutrient efficiency, polymer coated fertilizer with a controlled release behavior have been developed. This kind of fertilizer ensures a delayed release of nutrients to synchronize the nutrient supply with the demand of different crops. In the last decades, research focused primarily on semi-permeable polyurethane coatings, which remain in the soil for a long period after the complete solvation of the fertilizer core. Within the implementation of the new European Regulation Directive the replacement of non-degradable synthetic polymers by degradable coatings is necessary. It was, therefore, the objective of this study to develop a total biodegradable polymer (to CO2 and H2O) coating according to ISO 17556 and to compare the retarding effect of the biodegradable coatings with commercially available non-degradable products. To investigate the effect of ten selected coated urea fertilizer on the yield of annual ryegrass and maize, the fresh and dry mass, the percentage of total nitrogen and main nutrients were analyzed in greenhouse experiments in sixfold replications using near-infrared spectroscopy. For the experiments, a homogenized and air-dried loamy sand (Cambic Luvisol) was equipped with a basic fertilization of P, K, Mg and S. To investigate the effect of nitrogen level increase, three levels (80%, 100%, 120%) were established, whereas the impact of CRF granules was determined using a N-level of 100%. Additionally, leaching of NO3- from pots planted with annual ryegrass was examined to evaluate the retention capacity of urea by the polymer coating. For this, leachate from Kick-Brauckmann-Pots was collected daily and analyzed for total nitrogen, NO3- and NH4+ in twofold repetition once a week using near-infrared spectroscopy. We summarize from the results that the coated fertilizer have a clear impact on the yield of annual ryegrass and maize. Compared to the control, an increase of fresh and dry mass could be recognized. Partially, the non-degradable coatings showed a retarding effect for a longer period, which was however reflected by a lower fresh and dry mass. It was ascertained that the percentage of leached-out nitrate could be reduced markedly. As a conclusion, it could be pointed out that the impact of coated fertilizer of all polymer types might contribute to a reduction of negative environmental impacts in addition to their fertilizing effect.

Keywords: biodegradable polymers, coating, enhanced efficiency fertilizers, nitrate leaching

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Authors: Emmanuel Ogundimu, Esther Akinlabi, Mutiu Erinosho

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The aim of this paper is to study the effect of welding current on the microstructure and the mechanical properties. Material characterizations were conducted on a 6 mm thick plates of type-304 austenite stainless steel, welded by TIG welding process at two different welding currents of 150 A (Sample F3) and 170 A (Sample F4). The tensile strength and the elongation obtained from sample F4 weld were approximately 584 MPa and 19.3 %; which were higher than sample F3 weld. The average microhardness value of sample F4 weld was found to be 235.7 HV, while that of sample F3 weld was 233.4 HV respectively. Homogenous distribution of iron (Fe), chromium (Cr) and nickel (Ni) were observed at the welded joint of the two samples. The energy dispersive spectroscopy (EDS) analysis revealed that Fe, Cr, and Ni made up the composition formed in the weld zone. The optimum welding current of 170 A for TIG welding of type-304 austenite stainless steel can be recommended for high-tech industrial applications.

Keywords: microhardness, microstructure, tensile, MIG welding, process, tensile, shear stress TIG welding, TIG-MIG welding

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Authors: Gerd Wilsch, Tobias Guenther, Tobias Voelker

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In view of the ageing of vital infrastructure facilities, a reliable condition assessment of concrete structures is becoming of increasing interest for asset owners to plan timely and appropriate maintenance and repair interventions. For concrete structures, reinforcement corrosion induced by penetrating chlorides is the dominant deterioration mechanism affecting the serviceability and, eventually, structural performance. The determination of the quantitative chloride ingress is required not only to provide valuable information on the present condition of a structure, but the data obtained can also be used for the prediction of its future development and associated risks. At present, wet chemical analysis of ground concrete samples by a laboratory is the most common test procedure for the determination of the chloride content. As the chloride content is expressed by the mass of the binder, the analysis should involve determination of both the amount of binder and the amount of chloride contained in a concrete sample. This procedure is laborious, time-consuming, and costly. The chloride profile obtained is based on depth intervals of 10 mm. LIBS is an economically viable alternative providing chloride contents at depth intervals of 1 mm or less. It provides two-dimensional maps of quantitative element distributions and can locate spots of higher concentrations like in a crack. The results are correlated directly to the mass of the binder, and it can be applied on-site to deliver instantaneous results for the evaluation of the structure. Examples for the application of the method in the laboratory for the investigation of diffusion and migration of chlorides, sulfates, and alkalis are presented. An example for the visualization of the Li transport in concrete is also shown. These examples show the potential of the method for a fast, reliable, and automated two-dimensional investigation of transport processes. Due to the better spatial resolution, more accurate input parameters for model calculations are determined. By the simultaneous detection of elements such as carbon, chlorine, sodium, and potassium, the mutual influence of the different processes can be determined in only one measurement. Furthermore, the application of a mobile LIBS system in a parking garage is demonstrated. It uses a diode-pumped low energy laser (3 mJ, 1.5 ns, 100 Hz) and a compact NIR spectrometer. A portable scanner allows a two-dimensional quantitative element mapping. Results show the quantitative chloride analysis on wall and floor surfaces. To determine the 2-D distribution of harmful elements (Cl, C), concrete cores were drilled, split, and analyzed directly on-site. Results obtained were compared and verified with laboratory measurements. The results presented show that the LIBS method is a valuable addition to the standard procedures - the wet chemical analysis of ground concrete samples. Currently, work is underway to develop a technical code of practice for the application of the method for the determination of chloride concentration in concrete.

Keywords: chemical analysis, concrete, LIBS, spectroscopy

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Authors: A. Saurabh Singh, B. Raghvendra, C. Prabhakar Singh

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Solid Oxide Fuel Cells (SOFCs) are one of the most attractive electrochemical energy conversion systems, as these devices present a clean energy production, thus promising high efficiencies and low environmental impact. The electrodes are the main components that decisively control the performance of a SOFC. Conventional, anode materials (like Ni-YSZ) are operates at very high temperature. Therefore, cost-effective materials which operate at relatively lower temperatures are still required. In present study, we have synthesized La doped Strontium Titanate via solid state reaction route. The structural, microstructural and density of the pellet have been investigated employing XRD, SEM and Archimedes Principle, respectively. The electrical conductivity of the systems has been determined by impedance spectroscopy techniques. The electrical conductivity of the Lanthanum Strontium Titanate (LST) has been found to be higher than the composite Ni-YSZ system at 700 °C.

Keywords: IT-SOFC, LST, Lanthanum Strontium Titanate, electrical conductivity

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Authors: Darren A. Whitaker, Dan Palmer, Jens Wesholowski, James Flaherty, John Mack, Ahmad B. Albadarin, Gavin Walker

Abstract:

Traditional mechanosynthesis has been performed by either ball milling or manual grinding. However, neither of these techniques allow the easy application of process control. The temperature may change unpredictably due to friction in the process. Hence the amount of energy transferred to the reactants is intrinsically non-uniform. Recently, it has been shown that the use of Twin-Screw extrusion (TSE) can overcome these limitations. Additionally, TSE enables a platform for continuous synthesis or manufacturing as it is an open-ended process, with feedstocks at one end and product at the other. Several materials including metal-organic frameworks (MOFs), co-crystals and small organic molecules have been produced mechanochemically using TSE. The described advantages of TSE are offset by drawbacks such as increased process complexity (a large number of process parameters) and variation in feedstock flow impacting on product quality. To handle the above-mentioned drawbacks, this study utilizes UV-Vis spectrophotometry (InSpectroX, ColVisTec) as an online tool to gain real-time information about the quality of the product. Additionally, this is combined with real-time process information in an Advanced Process Control system (PharmaMV, Perceptive Engineering) allowing full supervision and control of the TSE process. Further, by characterizing the dynamic behavior of the TSE, a model predictive controller (MPC) can be employed to ensure the process remains under control when perturbed by external disturbances. Two reactions were studied; a Knoevenagel condensation reaction of barbituric acid and vanillin and, the direct amidation of hydroquinone by ammonium acetate to form N-Acetyl-para-aminophenol (APAP) commonly known as paracetamol. Both reactions could be carried out continuously using TSE, nuclear magnetic resonance (NMR) spectroscopy was used to confirm the percentage conversion of starting materials to product. This information was used to construct partial least squares (PLS) calibration models within the PharmaMV development system, which relates the percent conversion to product to the acquired UV-Vis spectrum. Once this was complete, the model was deployed within the PharmaMV Real-Time System to carry out automated optimization experiments to maximize the percentage conversion based on a set of process parameters in a design of experiments (DoE) style methodology. With the optimum set of process parameters established, a series of PRBS process response tests (i.e. Pseudo-Random Binary Sequences) around the optimum were conducted. The resultant dataset was used to build a statistical model and associated MPC. The controller maximizes product quality whilst ensuring the process remains at the optimum even as disturbances such as raw material variability are introduced into the system. To summarize, a combination of online spectral monitoring and advanced process control was used to develop a robust system for optimization and control of two TSE based mechanosynthetic processes.

Keywords: continuous synthesis, pharmaceutical, spectroscopy, advanced process control

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Authors: R. R. Galiev, I. I. Lykov, A. E. Shitikov, I. A. Bilenko

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Dual-comb interferometry is based on the mixing of two optical frequency combs with slightly different lines spacing which results in the mapping of the optical spectrum into the radio-frequency domain for future digitizing and numerical processing. The dual-comb approach enables diverse applications, including metrology, fast high-precision spectroscopy, and distance range. Ordinary frequency-modulated continuous-wave (FMCW) laser-based Light Identification Detection and Ranging systems (LIDARs) suffer from two main disadvantages: slow and unreliable mechanical, spatial scan and a rather wide linewidth of conventional lasers, which limits speed measurement resolution. Dual-comb distance measurements with Allan deviations down to 12 nanometers at averaging times of 13 microseconds, along with ultrafast ranging at acquisition rates of 100 megahertz, allowing for an in-flight sampling of gun projectiles moving at 150 meters per second, was previously demonstrated. Nevertheless, pump lasers with EDFA amplifiers made the device bulky and expensive. An alternative approach is a direct coupling of the laser to a reference microring cavity. Backscattering can tune the laser to the eigenfrequency of the cavity via the so-called self-injection locked (SIL) effect. Moreover, the nonlinearity of the cavity allows a solitonic frequency comb generation in the very same cavity. In this work, we developed a fully integrated, power-efficient, electrically driven dual-micro comb source based on the semiconductor lasers SIL to high-quality integrated Si3N4 microresonators. We managed to obtain robust 1400-1700 nm combs generation with a 150 GHz or 1 THz lines spacing and measure less than a 1 kHz Lorentzian withs of stable, MHz spaced beat notes in a GHz band using two separated chips, each pumped by its own, self-injection locked laser. A deep investigation of the SIL dynamic allows us to find out the turn-key operation regime even for affordable Fabry-Perot multifrequency lasers used as a pump. It is important that such lasers are usually more powerful than DFB ones, which were also tested in our experiments. In order to test the advantages of the proposed techniques, we experimentally measured a minimum detectable speed of a reflective object. It has been shown that the narrow line of the laser locked to the microresonator provides markedly better velocity accuracy, showing velocity resolution down to 16 nm/s, while the no-SIL diode laser only allowed 160 nm/s with good accuracy. The results obtained are in agreement with the estimations and open up ways to develop LIDARs based on compact and cheap lasers. Our implementation uses affordable components, including semiconductor laser diodes and commercially available silicon nitride photonic circuits with microresonators.

Keywords: dual-comb spectroscopy, LIDAR, optical microresonator, self-injection locking

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Authors: Salise Oktay, Nilgün Kizilcan, Başak Bengü

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At present, formaldehyde based adhesives such as urea formaldehyde (UF), melamine formaldehyde (MF), melamine – urea formaldehyde (MUF), etc. are mostly used in wood based panel industry because of their high reactivity, chemical versatility, and economic competitiveness. However, formaldehyde based wood adhesives are produced from non- renewable resources. Hence, there has been a growing interest in the development of environment friendly, economically competitive, bio-based wood adhesives in order to meet wood based panel industry requirements. In this study, as formaldehyde free adhesive, Mimosa tannin, starch, sugar based wood adhesivewas synthesized. Citric acid and tartaric acid were used as hardener for the resin system. Solid content, viscosity, and gel time analyzes of the prepared adhesive were performed in order to evaluate the adhesive processability. FTIR characterization technique was used to elucidate the chemical structures of the cured adhesivesamples. In order to evaluate the performance of the prepared bio-based resin formulation, particleboards were produced in a laboratory scale, and mechanical, physical properties of the boards were investigated. Besides, the formaldehyde contents of the boards were determined by using the perforator method. The obtained results revealed that the developed bio-based wood adhesive formulation can be a good potential candidate to use wood based panel industry with some developments.

Keywords: bio-based wood adhesives, mimosa tannin, corn starch, sugar, polycarboxyclic acid

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Authors: Josef Sepitka, Petr Vlcak, Tomas Horazdovsky, Vratislav Perina

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An ion implantation technique was used for designing the surface area of a titanium alloy and for irradiation-enhanced hardening of the surface. The Ti6Al4V alloy was treated by nitrogen ion implantation at fluences of 2·10¹⁷ and 4·10¹⁷ cm^-2 and at ion energy 90 keV. The depth distribution of the nitrogen was investigated by Rutherford Backscattering Spectroscopy. The gradient of mechanical properties was investigated by nanoindentation. The continuous measurement mode was used to obtain depth profiles of the indentation hardness and the reduced storage modulus of the modified surface area. The reduced storage modulus and the hardness increase with increasing fluence. Increased fluence shifts the peak of the mechanical properties as well as the peak of nitrogen concentration towards to the surface. This effect suggests a direct relationship between mechanical properties and nitrogen distribution.

Keywords: nitrogen ion implantation, titanium-based nanolayer, storage modulus, hardness, microstructure

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Authors: Devender Mandala, Paul Watts

Abstract:

Cis-Nucleosides mainly lamivudine (3TC) and emtricitabine (FTC) are an important tool in the treatment of Human immune deficiency virus (HIV), Hepatitis B virus (HBV) and Human T-Lymotropoic virus (HTLV). Lamivudine and emtricitabine are potent nucleoside analog reverse transcriptase inhibitors (nRTI). These two drugs are synthesized by a four-stage process from the starting materials: menthyl glyoxylate hydrate and 1,4-dithane-2,5-diol to produce the 5-hydroxy oxathiolane which upon acetylation with acetic anhydride to yield 5-acetoxy oxathiolane. Then glycosylation of this acetyl product with silyl protected nucleoside to produce the intermediate. The reduction of this intermediates can provide the final targets. Although there are several different methods reported for the synthesis of lamivudine and emtricitabine as a single enantiomer, we required an efficient route, which was suitable for large-scale synthesis to support the development of these compounds. In this process, we successfully prepared the intermediates of lamivudine and emtricitabine without using any solvents and catalyst, thus promoting the green synthesis. All the synthesized compound were confirmed by TLC, GC, Mass, NMR and 13C NMR spectroscopy.

Keywords: emtricitabine, green synthesis, lamivudine, nucleoside

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Authors: Augusto P. Andrade, Pedro L. Guedes, Pedro T. Da Silva, Liliane Ventura

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The present study evaluates the contribution of sunglasses frames as additional eye safety for ultraviolet backscatter light. Current sunglasses standards establish safe limits regarding lens transmittance in the 280 nm to 380 nm range. However, frames are additionally relevant in protecting the eyes from ultraviolet exposure. This study involves the use of a prototype that simulates backscattered light environments and quantifies the contribution of the frame as a function of the light that reaches the eye when wearing sunglasses. The prototype consists of an LED illuminated sphere, a mannequin head with optical sensors, and baseline and measurements are performed. A set of 29 samples was tested, and results show the variation of light blocking presented by different types of frames, ranging from 68% to 80%. This is still ongoing research. Prototype improvements for allowing albedo simulation, as well as the six types of sky simulation, are being implemented to show the intensity of UV light reaching the eye for several environments worldwide.

Keywords: sunglasses standards, sunglasses frame, ultraviolet protection, albedo

Procedia PDF Downloads 88