Search results for: gas chromatography-mass spectroscopy

Authors: Daniella R. Mulinari, Araujo J. F. Marina, Gabriella S. Lopes

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Natural fibers are used in polymer composites to improve mechanical properties, substituting inorganic reinforcing agents produced by non-renewable resources. The present study investigates the tensile, flexural and impact behaviors of palm fibers-high density polyethylene (HDPE) composite as a function of volume fraction. The surface of the fibers was modified by mercerization treatments to improve the wetting behavior of the apolar HDPE. The treatment characterization was obtained by scanning electron microscopy, X-Ray diffraction and infrared spectroscopy. Results evidence that a good adhesion interfacial between fibers-matrix causing an increase strength and modulus flexural as well as impact strength in the modified fibers/HDPE composites when compared to the pure HDPE and unmodified fibers reinforced composites.

Keywords: palm fibers, polymer composites, mechanical properties, high density polyethylene (HDPE)

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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: Noor Ul Ain Bhatti, M. Junaid Khan, Javed Ahmad, Murtaza Saleem, Shahid M. Ramay, Saadat A. Siddiqi

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Manganese oxide is being recently used as electrode material for rechargeable batteries. In this study, Al incorporated Mn₂O₃ compositions were synthesized to study the effect of Al doping on electrochemical performance of host material. Structural studies were carried out using X-ray diffraction analysis to confirm the phase stability and explore the lattice parameters, crystallite size, lattice strain, density and cell volume. Morphology and composition were analyzed using field emission scanning electron microscope and energy dispersive X-ray spectroscopy, respectively. Dynamic light scattering analysis was performed to observe the average particle size of the compositions. FTIR measurements exhibit the O-Al-O and O-Mn-O and Al-O bonding and with increasing the concentration of Al, the vibrational peaks of Mn-O become sharper. An enhanced electrochemical performance was observed in compositions with higher Al content.

Keywords: Mn2O3, electrode materials, energy storage and conversion, electrochemical performance

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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: M. H. Pazandeh, M. Doudi, S. Barahimi, L. Rahimzadeh Torabi

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The use of antibiotics is essential in reducing the occurrence of adverse effects and inhibiting the emergence of antibiotic resistance in microbial populations. The necessity for a novel methodology concerning local administration of antibiotics has arisen, with particular focus on dealing with localized infections prompted by bacterial colonization of medical devices or implant materials. Bioactive glasses (BG) are extensively employed in the field of regenerative medicine, encompassing a diverse range of materials utilized for drug delivery systems. In the present investigation, various drug carriers for imipenem and tetracycline, namely single systems BG/SnO2, BG/NiO with varying proportions of metal oxide, and nanocomposite BG/SnO2/NiO, were synthesized through the sol-gel technique. The antibacterial efficacy of the synthesized samples was assessed through the utilization of the disk diffusion method with the aim of neutralizing Staphylococcus aureus as the bacterial model. The current study involved the examination of the bioactivity of two samples, namely BG10SnO2/10NiO and BG20SnO2, which were chosen based on their heightened bacterial inactivation properties. This evaluation entailed the employment of two techniques: the measurement of the pH of simulated body fluid (SBF) solution and the analysis of the sample tablets through X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. The sample tablets were submerged in SBF for varying durations of 7, 14, and 28 days. The bioactivity of the composite bioactive glass sample was assessed through characterization of alterations in its surface morphology, structure, and chemical composition. This evaluation was performed using scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy, and X-ray diffraction spectroscopy. Subsequently, the sample was immersed in simulated liquids to simulate its behavior in biological environments. The specific body fat percentage (SBF) was assessed over a 28-day period. The confirmation of the formation of a hydroxyapatite surface layer serves as a distinct indicator of bioactivity. The infusion of antibiotics into the composite bioactive glass specimen was done separately, and then the release kinetics of tetracycline and imipenem were tested in simulated body fluid (SBF). Antimicrobial effectiveness against various bacterial strains have been proven in numerous instances using both melt and sol-gel techniques to create multiple bioactive glass compositions. An elevated concentration of calcium ions within a solution has been observed to cause an increase in the pH level. In aqueous suspensions, bioactive glass particles manifest a significant antimicrobial impact. The composite bioactive glass specimen exhibits a gradual and uninterrupted release, which is highly desirable for a drug delivery system over a span of 72 hours. The reduction in absorption, which signals the loss of a portion of the antibiotic during the loading process from the initial phosphate-buffered saline solution, indicates the successful bonding of the two antibiotics to the surfaces of the bioactive glass samples. The sample denoted as BG/10SnO2/10NiO exhibits a higher loading of particles compared to the sample designated as BG/20SnO2 in the context of bioactive glass. The enriched sample demonstrates a heightened bactericidal impact on the bacteria under investigation while concurrently preserving its antibacterial characteristics. Tailored bioactive glass that incorporates hydroxyapatite, with a regulated and efficient release of drugs targeting bacterial infections, holds promise as a potential framework for bone implant scaffolds following rigorous clinical evaluation, thereby establishing potential future biomedical uses. During the modification process, the introduction of metal oxides into bioactive glass resulted in improved antibacterial characteristics, particularly in the composite bioactive glass sample that displayed the highest level of efficiency.

Keywords: antibacterial, bioactive glasses, implant infections, multi drug resistant

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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: 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: G. Çelik Gül, F. Kurtuluş

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Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd₂Zr₃(MoO₄)₉, powder x-ray diffraction, solid state synthesis, zirconium molybdates

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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: Ayesha Irum, Sadia Mumtaz, Abdul Rehman, Iffat Naz, Safia Ahmed

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The present study was conducted to evaluate the potential applicability of biological trickling filter system for the treatment of simulated textile wastewater containing reactive azo dyes with bacterial consortium under non-sterile conditions. The percentage decolorization for the treatment of wastewater containing structurally different dyes was found to be higher than 95% in all trials. The stable bacterial count of the biofilm on stone media of the trickling filter during the treatment confirmed the presence, proliferation, dominance and involvement of the added microbial consortium in the treatment of textile wastewater. Results of physicochemical parameters revealed the reduction in chemical oxygen demand (58.5-75.1%), sulphates (18.9-36.5%), and phosphates (63.6-73.0%). UV-Visible and FTIR spectroscopy confirmed decolorization of dye containing wastewater was the ultimate consequence of biodegradation. Toxicological studies revealed the nontoxic nature of degradative metabolites.

Keywords: biodegradation, textile dyes, waste water, trickling filters

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Authors: Jadranka Blazhevska Gilev

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

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

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Authors: Humaira Khan, Mohsin Javed, Sammia Shahid

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The reinforced photocatalytic activity of graphene oxide (GO) along with composites of ZnO nanoparticles and copper-doped ZnO nanoparticles were studied by synthesizing ZnO and copper- doped ZnO nanoparticles by co-precipitation method. Zinc acetate and copper acetate were used as precursors, whereas graphene oxide was prepared from pre-oxidized graphite in the presence of H2O2.The supernatant was collected carefully and showed high-quality single-layer characterized by FTIR (Fourier Transform Infrared Spectroscopy), TEM (Transmission Electron Microscopy), SEM (Scanning Electron Microscopy), XRD (X-ray Diffraction Analysis), EDS (Energy Dispersive Spectrometry). The degradation of methylene blue as standard pollutant under UV-Visible irradiation gave results for photocatalytic activity of dopants. It could be concluded that shrinking of optical band caused by composites of Cu-dopped nanoparticles with GO enhances the photocatalytic activity.

Keywords: degradation, graphene oxide, photocatalysis, ZnO nanoparticles and copper-doped ZnO nanoparticles

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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: Samira Gharehkhani, Seyed Farid Seyed Shirazi, Abdolreza Gharehkhani, Hooman Yarmand, Ahmad Badarudin, Rushdan Ibrahim, Salim Newaz Kazi

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Nanocrystalline cellulose (NCC) were prepared by acid hydrolysis and ultrasound treatment of bleached Acacia mangium fibers. The obtained rod-shaped nanocrystals showed a uniform size. The results showed that NCC with high crystallinity can be obtained using 64 wt% sulfuric acid. The effect of synthesis condition was investigated. Different reaction times were examined to produce the NCC and the results revealed that an optimum reaction time has to be used for preparing the NCC. Morphological investigation was performed using the transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA) were performed. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments. The NCC suspension was homogeneous and stable and no sedimentation was observed for a long time.

Keywords: acid hydrolysis, nanocrystalline cellulose, nano material, reaction time

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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: Annu Sheokand, Vinay Kumar

Abstract:

Hydrogen sulfide (H₂S) detection is essential for environmental monitoring and industrial safety due to its high toxicity, even at low concentrations. This study explores the H₂S gas sensing properties of Cu-doped Fe₂O₃ materials derived from metal-organic frameworks (MOFs), which offer high surface area and controlled porosity for optimized gas sensing. The structural and morphological characteristics of the synthesized material were thoroughly analyzed using techniques such as X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), and UV-Vis Spectroscopy. The resulting sensor exhibited remarkable sensitivity and selectivity, achieving a detection limit at the ppb level for H₂S. The study indicates that Cu doping significantly enhances the gas sensing performance of Fe₂O₃ by introducing abundant active sites within the material. These enhanced sensing properties emphasize the potential of MOF-derived Cu-doped Fe₂O₃ as a highly effective material for H₂S gas sensors in various applications.

Keywords: detection limit, doping, MOF, sensitivity, sensor

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Authors: Amrei Voelkner, Nils Peters, Thomas Mannheim

Abstract:

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: Dilip K. Paul

Abstract:

The most popular mesoporous molecular sieves, Mobil Composition of Matter (MCM) are keenly studied by researchers because of these materials possess amorphous silica wall and have a long range of ordered framework with uniform mesopores. These materials also possess large surface area, which can be up to more than 1000 m2g−1. Herein the investigation is focused upon the synthesis and characterization of chromium and aluminum doped MCM-41 using XRD and FTIR. Acid-base properties of Cr-Al-MCM 41 was investigated by molecularly sensitive transmission FT-IR spectroscopy by adsorbing pyridine. In addition, these MCM nanomaterial was used to catalyze C-C bond formation from acetaldehyde adsorption. The assignment of all infrared peaks during adsorption of pyridine provided detail information on the presence of acid-base sites which in turn helped us to explain the roles of these in the condensation reaction of aldehyde. Reaction mechanisms of C-C bond formation is therefore explored to shed some light on this elusive reaction detail.

Keywords: mesoporous nanomaterial, MCM 41, FTIR studies, acid-base studies

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Authors: Emmanuel Ogundimu, Esther Akinlabi, Mutiu Erinosho

Abstract:

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

Abstract:

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

Procedia PDF Downloads 103

Authors: Surjyakanta Rana, Sreekantha B. Jonnalagadda

Abstract:

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

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

Procedia PDF Downloads 373