Search results for: NMR spectroscopy

Authors: Priya Arora, Jaspreet K. Rajput

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Superparamagnetism has accelerated the research and use of more economical and ecological magnetically separable catalysts due to their more efficient isolation by response to an applied magnetic field. Magnetite nanomaterials coated by SiO2 shell have received a great deal of focus in the last decades as it provides high stability and also easy further surface functionalization depending upon the application. In this protocol, Fe3O4 magnetic nanoparticles have been synthesized by co-precipitation combined with sonication method. Further, Fe3O4 superparamagnetic nanoparticles have been functionalized by various moieties to serve as efficient catalysts for multicomponent reactions. The functionalized nanoparticles were characterized by techniques like Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET) surface area analysis. The as prepared nanocatalysts can be reused for several times without any significant loss in its activity. The utilization of magnetic nanoparticles as catalysts for this reaction is one approach i.e. green, inexpensive, facile and widely applicable.

Keywords: functionalized, magnetite, multicomponent reactions, superparamagnetic

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Authors: Csilla Dudás, Éva Böszörményi, Bence Kutus, István Pálinkó, Pál Sipos

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In this study the behavior of alpha-D-isosaccharinate (2-hydroxymethyl-3-deoxy-D-erythro-pentonate, ISA−) in alkaline medium in the presence of calcium was studied. At first the Ca–ISA system was studied by Ca-ion selective electrode (Ca-ISE) in neutral medium at T = 25 °C and I = 1 M NaCl to determine the formation constant of the CaISA+ monocomplex, which was found to be logK = 1.01 ± 0.01 for the reaction of Ca2+ + ISA– = CaISA+. In alkaline medium pH potentiometric titrations were carried out to determine the composition and stability constant of the complex(es) formed. It was found that in these systems above pH = 12.5 the predominant species is the CaISAOH complex. Its formation constant was found to be logK = 3.04 ± 0.05 for the reaction of Ca2+ + ISA– + H2O = CaISAOH + H+ at T = 25 °C and I = 1 M NaCl. Solubility measurements resulted in data consistent with those of the potentiometric titrations. Temperature dependent NMR spectra showed that the slow exchange range between the complex and the free ligand is below 5 °C. It was also showed that ISA– acts as a multidentate ligand forming macrochelate Ca-complexes. The structure of the complexes was determined by using ab initio quantum chemical calculations.

Keywords: Ca-ISE potentiometry, calcium complexes, isosaccharinate ion, NMR spectroscopy, pH potentiometry

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Authors: Neşe Taşci, Soner Çubuk, Ece Kök Yetimoğlu, M. Vezir Kahraman

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Bisphenol-A (BPA), 2,2-bis(4-hydroxyphenly)propane, is one of the highest usage volume chemicals in the world. Studies showed that BPA maybe has negative effects on the central nervous system, immune and endocrine systems. Several of analytical methods for the analysis of BPA have been reported including electrochemical processes, chemical oxidation, ozonization, spectrophotometric, chromatographic techniques. Compared with other conventional analytical techniques, optic sensors are reliable, providing quick results, low cost, easy to use, stands out as a much more advantageous method because of the high precision and sensitivity. In this work, a new photocured polymeric fluorescence sensor was prepared and characterized for Bisphenol-A (BPA) analysis. Characterization of the membrane was carried out by Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR) and Scanning Electron Microscope (SEM) techniques. The response characteristics of the sensor including dynamic range, pH effect and response time were systematically investigated. Acknowledgment: This work was supported by the Scientific and Technological Research Council of Turkey (TUBITAK) under Grant 115Y469.

Keywords: bisphenol-a, fluorescence, photopolymerization, polymeric sensor

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Authors: Bayan Alqassem, Israa A. Othman, Mohammed Abu Haija, Fawzi Banat

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The treatment of wastewater from highly toxic pollutants is one of the most challenging issues for humanity. In this study, the advanced oxidation process (AOP) was employed to study the catalytic degradation of phenol using different ferrite catalysts which are CoFe₂O₄, CrFe₂O₄, CuFe₂O₄, MgFe₂O₄, MnFe₂O₄, NiFe₂O₄ and ZnFe₂O₄. The ferrite catalysts were prepared via sol-gel and co-precipitation methods. Different ferrite composites were also prepared either by varying the metal ratios or incorporating chemically reduced graphene oxide in the ferrite cluster. The effect of phosphoric acid treatment on the copper ferrite activity. All of the prepared catalysts were characterized using infrared spectroscopy (IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The ferrites catalytic activities were tested towards phenol degradation using high performance liquid chromatography (HPLC). The experimental results showed that ferrites prepared through sol-gel route were more active than those of the co-precipitation method towards phenol degradation. In both cases, CuFe₂O₄ exhibited the highest degradation of phenol compared to the other ferrites. The photocatalytic properties of the ferrites were also investigated.

Keywords: ferrite catalyst, ferrite composites, phenol degradation, photocatalysis

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Authors: Delele Worku Ayele, Bing-Joe Hwang

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A method that does not employ hot injection techniques has been developed for the size-tunable synthesis of high-quality CdSe quantum dots (QDs) with a zinc blende structure. In this environmentally benign synthetic route, which uses relatively less toxic precursors, solvents, and capping ligands, CdSe QDs that absorb visible light are obtained. The size of the as-prepared CdSe QDs and, thus, their optical properties can be manipulated by changing the microwave reaction conditions. The QDs are characterized by XRD, TEM, UV-vis, FTIR, time-resolved fluorescence spectroscopy, and fluorescence spectrophotometry. In this approach, the reaction is conducted in open air and at a much lower temperature than in hot injection techniques. The use of microwaves in this process allows for a highly reproducible and effective synthesis protocol that is fully adaptable for mass production and can be easily employed to synthesize a variety of semiconductor QDs with the desired properties. The possible application of the as-prepared CdSe QDs has been also assessed using deposition on TiO2 films.

Keywords: CdSe QDs, Na2SeSO3, microwave (MW), oleic acid, mass production, average life time

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Authors: Farzana Majid, Mahwish Bashir, Ammara, Attia Falak

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Zirconia nanoparticles have gained significant attention due to their excellent mechanical strength, thermal properties, biocompatibility, and catalytic activity. Tetragonal zirconia holds the greatest efficacy for surgical implants and coatings when it comes to the three zirconia phases (monoclinic, tetragonal, and cubic). However, its stability at higher temperatures and transformation to the monoclinic phase upon cooling are challenging. In this research, zirconia nanoparticles were prepared using microwave-assisted sol-gel method with varying microwave powers (100 W, 300 W, 500 W, 700 W, & 900 W). Organic stabilizing agent, i.e., eggshell powder, was used to stabilize the tetragonal phase. Fourier transform infrared spectroscopy (FTIR) confirmed the phase-pure tetragonal zirconia, corroborating the XRD data. Optical properties, including the optical bandgap, were studied using UV/Visible and PL spectroscopies. The synthesized ZrO2 nanoparticles exhibited excellent photocatalytic degradation efficiency in the degradation of methylene blue (MB) dye under UV irradiation. The findings demonstrate the potential of these ZrO2 nanoparticles as a viable alternative photocatalyst for the efficient degradation of various dyes in contaminated water.

Keywords: zirconia nanoparticles, sol-gel, photocataylsis, wter purification

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Authors: Woei-Shyan Lee, Shuo-Ling Chang

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The nanoindentation behaviour and phase transformation of annealed single-crystal silicon wafers are examined. The silicon specimens are annealed at temperatures of 250, 350 and 450ºC, respectively, for 15 minutes and are then indented to maximum loads of 30, 50 and 70 mN. The phase changes induced in the indented specimens are observed using transmission electron microscopy (TEM) and micro-Raman scattering spectroscopy (RSS). For all annealing temperatures, an elbow feature is observed in the unloading curve following indentation to a maximum load of 30 mN. Under higher loads of 50 mN and 70 mN, respectively, the elbow feature is replaced by a pop-out event. The elbow feature reveals a complete amorphous phase transformation within the indented zone, whereas the pop-out event indicates the formation of Si XII and Si III phases. The experimental results show that the formation of these crystalline silicon phases increases with an increasing annealing temperature and indentation load. The hardness and Young’s modulus both decrease as the annealing temperature and indentation load are increased.

Keywords: nanoindentation, silicon, phase transformation, amorphous, annealing

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Authors: F. Chigondo, G. Chitabati

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Hexavalent chromium is toxic and is widely used in many industries hence efficient and economical methods must be explored to remove the chromium(VI) from the environment. The removal of Cr (VI) from aqueous solutions onto polyaniline coated maize tassel was studied in batch mode at varying initial metal concentrations, adsorbent doses, pH and contact times. The residual Cr (VI) concentrations before and after adsorption were analyzed by Ultraviolet–visible spectroscopy. FTIR analysis of the polyaniline coated maize tassel showed the presence of C=C, C=N, C-H, C-N and N-H groups. Adsorption conditions were deduced to be pH of 2, adsorbent dosage 1g/L, Cr(VI) initial concentration of 40mg/L contact time of 150 minutes and agitation speed of 140rpm. Data obtained fitted best to the Langmuir isotherm (R2 = 0.972) compared to the Freundlich isotherm (R2 0.671. The maximum adsorption capacity was found to be 125mg/L. Correlation coefficients for pseudo first order and pseudo second order were 0.952 and 0.971 respectively. The adsorption process followed the pseudo-second order kinetic model. The studied polyaniline coated maize tassel can therefore be used as a promising adsorbent for the removal of Cr (VI) ion from aqueous solution.

Keywords: polyaniline-coated, maize tassels, adsorption, hexavalent chromium

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Authors: Ria Ghosh, Soumendra Singh, Dipanjan Mukherjee, Susmita Mondal, Monojit Das, Uttam Pal, Aniruddha Adhikari, Aman Bhushan, Surajit Bose, Siddharth Sankar Bhattacharyya, Debasish Pal, Tanusri Saha-Dasgupta, Maitree Bhattacharyya, Debasis Bhattacharyya, Asim Kumar Mallick, Ranjan Das, Samir Kumar Pal

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Drug delivery to a target without adverse effects is one of the major criteria for clinical use. Herein, we have made an attempt to explore the delivery efficacy of SDS surfactant in a monomer and micellar stage during the delivery of the model drug, Toluidine Blue (TB) from the micellar cavity to DNA. Molecular recognition of pre-micellar SDS encapsulated TB with DNA occurs at a rate constant of k1 ~652 s 1. However, no significant release of encapsulated TB at micellar concentration was observed within the experimental time frame. This originated from the higher binding affinity of TB towards the nano-cavity of SDS at micellar concentration which does not allow the delivery of TB from the nano-cavity of SDS micelles to DNA. Thus, molecular recognition controls the extent of DNA recognition by TB which in turn modulates the rate of delivery of TB from SDS in a concentration-dependent manner.

Keywords: DNA, drug delivery, micelle, pre-micelle, SDS, toluidine blue

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Authors: Esra Alveroglu Durucu, Kenan Koc

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In this study, we synthesized and characterized nano-sized Poly- N-isopropylacrylamide (PNIPAM) hydrogels. N-isopropylacrylamide (NIPAM) micro and macro gels are known as a thermosensitive colloidal structure, and they respond to changes in the environmental conditions such as temperature and pH. Here, nano-sized gels were synthesized via precipitation copolymerization method. N,N-methylenebisacrylamide (BIS) and ammonium persulfate APS were used as crosslinker and initiator, respectively. 8-Hydroxypyrene-1,3,6- trisulfonic Acid (Pyranine, Py) molecules were used for arranging the particle size and thus physical properties of the nano-sized hydrogels. Fluorescence spectroscopy, atomic force microscopy and light scattering methods were used for characterizing the synthesized hydrogels. The results show that the gel size was decreased with increasing amount of ionic molecule from 550 to 140 nm due to the electrostatic behavior of the ionic side groups of pyranine. Light scattering experiments demonstrate that lower critical solution temperature (LCST) of the gels shifts to the lower temperature with decreasing size of gel due to the hydrophobicity–hydrophilicity balance of the polymer chains.

Keywords: hydrogels, lower critical solution temperature, nanogels, poly(n-isopropylacrylamide)

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Authors: E. Kam, G. Karahan, H. Aslıyuksek, A. Bozkurt

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This study aims to determine the natural radioactivity levels in some foodstuffs produced in Turkey. For this purpose, 48 different foods samples were collected from different land parcels throughout the country. All samples were analyzed to designate both gross alpha and gross beta radioactivities and the radionuclides’ concentrations. The gross alpha radioactivities were measured as below 1 Bq kg^-1 in most of the samples, some of them being due to the detection limit of the counting system. The gross beta radioactivity levels ranged from 1.8 Bq kg^-1 to 453 Bq kg^-1, larger levels being observed in leguminous seeds while the highest level being in haricot bean. The concentrations of natural radionuclides in the foodstuffs were investigated by the method of gamma spectroscopy. High levels of ⁴⁰K were measured in all the samples, the highest activities being again in leguminous seeds. Low concentrations of ²³⁸U and ²²⁶Ra were found in some of the samples, which are comparable to the reported results in the literature. Based on the activity concentrations obtained in this study, average annual effective dose equivalents for the radionuclides ²²⁶Ra, ²³⁸U, and ⁴⁰K were calculated as 77.416 µSv y^-1, 0.978 µSv y^-1, and 140.55 µSv y^-1, respectively.

Keywords: foods, radioactivity, gross alpha, gross beta, annual equivalent dose, Turkey

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Authors: Jose Alberto Duarte Moller, Cynthia Deisy Gomez Esparza

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The cobalt-titanium system was grown as thin films in an INTERCOVAMEX V3 sputtering system, equipped with four magnetrons assisted by DC pulsed and direct DC. A polished highly oriented (400) silicon wafer was used as substrate and the growing temperature was 500 oC. Xray Absorption Spectroscopy experiments were carried out in the SSRL in the 4-3 beam line. The Extenden X-Ray Absorption Fine Structure spectra have been numerically processed by WINXAS software from the background subtraction until the normalization and FFT adjustment. Analyzing the absorption spectra of cobalt in the CoTi2 phase we can appreciate that they agree in energy with the reference spectra that corresponds to the CoO, which indicates that the valence where upon working is Co2+. The RDF experimental results were then compared with those RDF´s generated theoretically by using FEFF software, from a model compound of CoTi2 phase obtained by XRD. The fitting procedure is a highly iterative process. Fits are also checked in R-space using both the real and imaginary parts of Fourier transform. Finally, the presence of overlapping coordination shells and the correctness of the assumption about the nature of the coordinating atom were checked.

Keywords: XAS, EXAFS, FEFF, CoTi

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Authors: M. Yildirim, A. S. Kipcak, F. T. Senberber, M. O. Asensio, E. M. Derun, S. Piskin

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Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8•4H2O) was synthesized as best.

Keywords: hydrothermal synthesis, potassium borate, potassium nitrate, santite

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Authors: Azyuni Aziz, Syed A. Malik, Shahrul Kadri Ayop, Fatin Hana Naning

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Currently, organic-inorganic hybrid thin films have attracted researchers to explore them, where these thin films can give a lot of benefits. Hybrid thin films are thin films that consist of inorganic and organic materials. Inorganic and organic materials give high efficiency and low manufacturing cost in some applications such as solar cells application, furthermore, organic materials are environment-friendly. In this study, poly (3-hexylthiophene) was choosing as organic material which combined with inorganic nanoparticles, Cadmium Sulfide (CdS) quantum dots. Samples were prepared using new technique, Angle Lifting Deposition (ALD) at different weight percentage. All prepared samples were then characterized by Field Emission Scanning Electron Microscopy (FESEM) with Energy-dispersive X-ray spectroscopy (EDX) and Atomic Force Microscopy (AFM) to study surface of samples and determine their surface roughness. Results show that these inorganic nanoparticles have affected the surface of samples and surface roughness of samples increased due to increasing of weight percentage of CdS in the thin films samples.

Keywords: AFM, CdS, FESEM-EDX, hybrid thin films, P3HT

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Authors: Ellie Fini, Mahour Parast, Daniel Oldham, Shahrzad Hosseinnezhad

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This paper investigates the relationship between molecular species of four different bio-based adhesives (made from Swine Manure, Miscanthus Pellet, Corn Stover, and Wood Pellet) and their rheological behavior before and after they undergo extensive oxidative aging. To study the effect of oxidative aging on the chemical structure of bio-adhesives, Infrared Attenuated Total Reflectance Spectroscopy (Fourier transform infrared) was utilised. In addition, a Drop Shape Analyser, Rotational Viscometer, and Dynamic Shear Rheometer were used to evaluate the surface properties and rheological behaviour of each bio-adhesive. Overall, bio-adhesives were found to be significantly different in terms of their ageing characteristics. Accordingly, their surface and rheological properties were found to be ranked differently before and after ageing. The results showed that the bio-adhesive from swine manure is less susceptible to aging compared to plant-based bio-oils. This can be further attributed to the chemical structure and the high lipid contents of the bio-adhesive from swine manure, making it less affected by oxidative ageing.

Keywords: bio-adhesive, rheology, bio-mass, material genome

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Authors: P. Chihomvu, P. Stegmann, M. Pillay

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Pollution of the Klip River has caused microorganisms inhabiting it to develop protective survival mechanisms. This study isolated and characterized the heavy metal resistant bacteria in the Klip River. Water and sediment samples were collected from six sites along the course of the river. The pH, turbidity, salinity, temperature and dissolved oxygen were measured in-situ. The concentrations of six heavy metals (Cd, Cu, Fe, Ni, Pb, and Zn) of the water samples were determined by atomic absorption spectroscopy. Biochemical and antibiotic profiles of the isolates were assessed using the API 20E® and Kirby Bauer Method. Growth studies were carried out using spectrophotometric methods. The isolates were identified using 16SrDNA sequencing. The uppermost part of the Klip River with the lowest pH had the highest levels of heavy metals. Turbidity, salinity and specific conductivity increased measurably at Site 4 (Henley on Klip Weir). MIC tests showed that 16 isolates exhibited high iron and lead resistance. Antibiotic susceptibility tests revealed that the isolates exhibited multi-tolerances to drugs such as tetracycline, ampicillin, and amoxicillin.

Keywords: Klip River, heavy metals, resistance, 16SrDNA

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Authors: A.G. S. Aldajani, N. Smida, M. G. Althobaiti, B. Zaidi

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In order to exploit the good electrical properties of anthracene and the excellent properties of fluorescein, new hybrid material has been synthesized (An-Fl). Current-voltage measurements were done on a new single-layer ITO/An-FL/Al device of typically 100 nm thickness. Atypical diode behavior is observed with a turn-on voltage of 4.4 V, a dynamic resistance of 74.07 KΩ and a rectification ratio of 2.02 due to unbalanced transport. Results show also that the current-voltage characteristics present three different regimes of the power-law (J~Vᵐ) for which the conduction mechanism is well described with space-charge-limited current conduction mechanism (SCLC) with a charge carrier mobility of 2.38.10⁻⁵cm2V⁻¹S⁻¹. Moreover, the electrical transport properties of this device have been carried out using a dependent frequency study in the range (50 Hz–1.4 MHz) for different applied biases (from 0 to 6 V). At lower frequency, the σdc values increase with bias voltage rising, supporting that the mobile ion can hop successfully to its nearest vacant site. From σac and impedance measurements, the equivalent electrical circuit is evidenced, where the conductivity process is coherent with an exponential trap distribution caused by structural defects and/or chemical impurities.

Keywords: semiconducting polymer, conductivity, SCLC, impedance spectroscopy

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Authors: Thabelo Nelushi, Michael Scurrell, Tumelo Seadira

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Global warming is one of the most important environmental issues which arise from occurrence of gases such as carbon dioxide (CO2) and methane (CH4) in the atmosphere. Exposure to these greenhouse gases results in health risk. Hydrogen is regarded as an alternative energy source which is a clean energy carrier for the future. There are different methods to produce hydrogen such as steam reforming, coal gasification etc., however the challenge with these processes is that they emit CO and CO2 gases and are costly. Photocatalytic reforming is a substitute process which is fascinating due to the combination of solar energy and renewable sources and the use of semiconductor materials such as catalysts. TiO2 is regarded as the most promising catalysts. TiO2 nanoparticles prepared by hydrothermal method and Ag/TiO2 are being investigated for photocatalytic production of hydrogen from butanol. The samples were characterized by raman spectroscopy, TEM/SEM, XRD, XPS, EDAX, DRS and BET surface area. 2 wt% Ag-doped TiO2 nanoparticle showed enhanced hydrogen production compared to a non-doped TiO2. The results of characterization and photoactivity shows that TiO2 nanoparticles play a very important role in producing high hydrogen by utilizing solar irradiation.

Keywords: butanol, hydrogen production, silver particles, TiO2 nanoparticles

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Authors: Payam Hayati, Fateme Firoozbakht, Gholamhassan Azimi, Shahram Tangestaninejad

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The synthesis of a photocatalytic adsorbent involved the integration of carbon dots (CD) into a metal-organic framework (MOF) of MIL-88B(Fe) using the solvothermal technique. Characterization of the resulting CD@MIL-88B(Fe) was conducted using various analytical methods, including X-ray-based microscopic and spectroscopic techniques, electrochemical impedance spectroscopy, UV–Vis, FT-IR, DRS, TGA, and photoluminescence (PL) analysis. The adsorbent demonstrated significant photocatalytic activity, achieving up to 92% and 90% removal of amphotericin B (AmB) and naproxen (Nap) from aqueous solutions under visible light, with an RSD value of around 5%. The study explored the factors influencing the degradation of pharmaceuticals and determined the optimal conditions for the process, including pH values of 3 and 4 for AmB and Nap, a photocatalyst concentration of 0.2 g L-1, and an H2O2 concentration ranging from 40 to 50 mM. Reactive oxidative species such as ⋅OH and ⋅O2 were identified through the examination of different scavengers. Additionally, the adsorption isotherm and kinetic studies revealed that the synthesized photocatalyst functions as an effective adsorbent, with maximum adsorption capacities of 42.5 and 121.5 mg g-1 for AmB and Nap, while also serving as a photocatalytic agent for removal purposes.

Keywords: fenton-like degradation, metal-organic frameworks, heterogenous photocatalysts, naproxen

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Authors: Fatima Melit, Nedjemeddine Bounar

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Polycrystalline samples of Ce1-xMxO2-δ (x=0.1, 0.15, 0.2)(M=Gd, Y) were prepared by solid-state chemical reaction from mixtures of pre-dried oxides powders of CeO2, Gd2O3 and Y2O3 in the appropriate stoichiometric ratio to explore their use as solid electrolytes for intermediate temperature solid oxide fuel cells (IT-SOFCs). Their crystal structures and ionic conductivities were characterised by X-ray powder diffraction (XRD) and AC complex impedance spectroscopy (EIS). The XRD analyses confirm that all the resulting synthesised co-doped cerium oxide powders are single-phase and crystallise in the cubic structure system with the space group Fm3m. On the one hand, the lattice parameter (a ) of the phases increases with increasing Gd content; on the other hand, with increasing Y-substitution rate, the latter decreases. The results of complex impedance conductivity measurements have shown that doping has a remarkable effect on conductivity. The co-doped cerium phases showed significant ionic conductivity values, making these materials excellent candidates for solid oxide electrolytes at intermediate temperatures.

Keywords: electrolyte, Ceria, X-ray diffraction, EIS, SEM, SOFC

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Authors: A. Kaibi, A. Guittoum, M. Hemmous, D. Martínez-Blanco, P. Gorria, J. A. Blanco, M. Kechouane

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The present work deals with the effect of Si content on the physical properties of nanostructured (Ni75Fe25)100-x Six (x=0, 3.5, 6.5, 9, 12, and 15 at %) powders elaborated by mechanical alloying for a milling time of 96 h. The microstructure, hyperfine, and magnetic properties of the powders were investigated as a function of Si content by means of X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Mössbauer Spectroscopy, and Vibrating Sample magnetometry (VSM). From XRD spectra, the formation of FCC disordered Ni (Fe,Si) solid solution was evidenced after 96 h. As Si content increases, the lattice parameter and the grain size decrease (from ~28 to 15 nm), while the microstrain level decreases from 0.98% to 0.65%. From SEM micrographs, we showed that powder particles become round in shape and decrease in size with increasing Si content. For all Si content, the adjustment of Mössbauer spectra confirmed the formation of a disordered ferromagnetic NiFeSi phase. From hysteresis curves, we have extracted the values of saturation magnetization and coercive field for all powders. The evolution of Ms and Hc as a function of Si content will be discussed.

Keywords: nanostructured powders, (Ni75Fe25)100-xSix alloy, microstructure, magnetic properties

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Authors: Irina Mizeva, Elena Potapova, Viktor Dremin, Mikhail Mezentsev, Valeri Shupletsov

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The local tissue perfusion is regulated by the microvascular tone which is under the control of a number of physiological mechanisms. Laser Doppler flowmetry (LDF) together with wavelet analyses is the most commonly used technique to study the regulatory mechanisms of cutaneous microcirculation. External factors such as temperature, local pressure of the probe on the skin, etc. influence on the blood flow characteristics and are used as physiological tests to evaluate microvascular regulatory mechanisms. Local probe pressure influences on the microcirculation parameters measured by optical methods: diffuse reflectance spectroscopy, fluorescence spectroscopy, and LDF. Therefore, further study of probe pressure effects can be useful to improve the reliability of optical measurement. During pressure tests variation of the mean perfusion measured by means of LDF usually is estimated. An additional information concerning the physiological mechanisms of the vascular tone regulation system in response to local pressure can be obtained using spectral analyses of LDF samples. The aim of the present work was to develop protocol and algorithm of data processing appropriate for study physiological response to the local pressure test. Involving 6 subjects (20±2 years) and providing 5 measurements for every subject we estimated intersubject and-inter group variability of response of both averaged and oscillating parts of the LDF sample on external surface pressure. The final purpose of the work was to find special features which further can be used in wider clinic studies. The cutaneous perfusion measurements were carried out by LAKK-02 (SPE LAZMA Ltd., Russia), the skin loading was provided by the originally designed device which allows one to distribute the pressure around the LDF probe. The probe was installed on the dorsal part of the distal finger of the index figure. We collected measurements continuously for one hour and varied loading from 0 to 180mmHg stepwise with a step duration of 10 minutes. Further, we post-processed the samples using the wavelet transform and traced the energy of oscillations in five frequency bands over time. Weak loading leads to pressure-induced vasodilation, so one should take into account that the perfusion measured under pressure conditions will be overestimated. On the other hand, we revealed a decrease in endothelial associated fluctuations. Further loading (88 mmHg) induces amplification of pulsations in all frequency bands. We assume that such loading leads to a higher number of closed capillaries, higher input of arterioles in the LDF signal and as a consequence more vivid oscillations which mainly are formed in arterioles. External pressure higher than 144 mmHg leads to the decrease of oscillating components, after removing the loading very rapid restore of the tissue perfusion takes place. In this work, we have demonstrated that local skin loading influence on the microcirculation parameters measured by optic technique; this should be taken into account while developing portable electronic devices. The proposed protocol of local loading allows one to evaluate PIV as far as to trace dynamic of blood flow oscillations. This study was supported by the Russian Science Foundation under project N 18-15-00201.

Keywords: blood microcirculation, laser Doppler flowmetry, pressure-induced vasodilation, wavelet analyses blood

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Authors: Jinyoung Kim, Jinuk Kwon, Haksoo Han

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Polyimide is widely used in electronic industries, and heat dissipation of polyimide film is important for its application in electric devices for high-temperature resistance heat dissipation film. In this study, we demonstrated a new way to increase heat dissipating rate by adding carbon black as filler. This type of polyimide composite film was produced by pyromellitic dianhydride (PMDA) and 4,4’-oxydianiline (ODA). Carbon black (CB) is added in different loading, shows increasing heat dissipation rate for increase of Carbon black. The polyimide-carbon black composite film is synthesized with high dissipation rate to ~8W∙m−1K−1. Its high thermal decomposition temperature and glass transition temperature were maintained with carbon filler verified by thermogravimetric analysis (TGA) and differential scanning calorimetric (DSC), the polyimidization reaction of polyi(amide-mide) was confirmed by Fourier transform infrared spectroscopy (FT-IR). The polyimide composite film with carbon black with high heat dissipating rate could be used in various applications such as computers, mobile phone industries, integrated circuits, coating materials, semiconductor etc.

Keywords: polyimide, heat dissipation, electric device, filler

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Authors: Irene Carmagnola, Valeria Chiono, Sandra Pacharra, Jochen Salber, Sean McMahon, Chris Lovell, Pooja Basnett, Barbara Lukasiewicz, Ipsita Roy, Xiang Zhang, Gianluca Ciardelli

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Thrombosis and restenosis after stenting procedure can be prevented by promoting fast stent wall endothelialisation. It is well known that surface functionalisation with antifouling molecules combining with extracellular matrix proteins is a promising strategy to design biomimetic surfaces able to promote fast endothelialization. In particular, REDV has gained much attention for the ability to enhance rapid endothelialization due to its specific affinity with endothelial cells (ECs). In this work, a two-step plasma treatment was performed to polymerize a thin layer of acrylic acid, used to subsequently graft PEGylated-REDV and polyethylene glycol (PEG) at different molar ratio with the aim to selectively promote endothelial cell adhesion avoiding platelet activation. PEGylate-REDV was provided by Biomatik and it is formed by 6 PEG monomer repetitions (Chempep Inc.), with an NH2 terminal group. PEG polymers were purchased from Chempep Inc. with two different chain lengths: m-PEG6-NH2 (295.4 Da) with 6 monomer repetitions and m-PEG12-NH2 (559.7 Da) with 12 monomer repetitions. Plasma activation was obtained by operating at 50W power, 5 min of treatment and at an Ar flow rate of 20 sccm. Pure acrylic acid (99%, AAc) vapors were diluted in Ar (flow = 20 sccm) and polymerized by a pulsed plasma discharge applying a discharge RF power of 200 W, a duty cycle of 10% (on time = 10 ms, off time = 90 ms) for 10 min. After plasma treatment, samples were dipped into an 1-(3-dimethylaminopropyl)-3- ethylcarbodiimide (EDC)/N-hydroxysuccinimide (NHS) solution (ratio 4:1, pH 5.5) for 1 h at 4°C and subsequently dipped in PEGylate-REDV and PEGylate-REDV:PEG solutions at different molar ratio (100 μg/mL in PBS) for 20 h at room temperature. Surface modification was characterized through physico-chemical analyses and in vitro cell tests. PEGylated-REDV peptide and PEG were successfully bound to the carboxylic groups that are formed on the polymer surface after plasma reaction. FTIR-ATR spectroscopy, X -ray Photoelectron Spectroscopy (XPS) and contact angle measurement gave a clear indication of the presence of the grafted molecules. The use of PEG as a spacer allowed for an increase in wettability of the surface, and the effect was more evident by increasing the amount of PEG. Endothelial cells adhered and spread well on the surfaces functionalized with the REDV sequence. In conclusion, a selective coating able to promote a new endothelial cell layer on polymeric stent surface was developed. In particular, a thin AAc film was polymerised on the polymeric surface in order to expose –COOH groups, and PEGylate-REDV and PEG were successful grafted on the polymeric substrates. The REDV peptide demonstrated to encourage cell adhesion with a consequent, expected improvement of the hemocompatibility of these polymeric surfaces in vivo. Acknowledgements— This work was funded by the European Commission 7th Framework Programme under grant agreement number 604251- ReBioStent (Reinforced Bioresorbable Biomaterials for Therapeutic Drug Eluting Stents). The authors thank all the ReBioStent partners for their support in this work.

Keywords: endothelialisation, plasma treatment, stent, surface functionalisation

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Authors: Fernando G. Torres, Omar P. Troncoso

Abstract:

Starch is a highly biocompatible, non-toxic, and biodegradable polymer. It is widely used in biomedical applications, including drug delivery systems and tissue engineering scaffolds. Curcumin, a phenolic compound found in the dried root of Curcuma longa, has been used as a nutritional supplement due to its antimicrobial, anti-inflammatory, and antioxidant effects. However, the major problem with ingesting curcumin by itself is its poor bioavailability due to its poor absorption and rapid metabolism. In this study, we report a novel methodology to prepare starch nanoparticles loaded with curcumin. The nanoparticles were synthesized via nanoprecipitation of starch granules extracted from native Andean potatoes (Solanum tuberosum ssp. and Andigena var Huamantanga varieties). The nanoparticles were crosslinked and stabilized by using sodium tripolyphosphate and Tween®80, respectively. The characterization of the nanoparticles loaded with curcumin was assessed by Fourier Transform Infrared Spectroscopy, Dynamic Light Scattering, Zeta potential, and Differential scanning calorimetry. UV-vis spectrophotometry was used to evaluate the loading efficiency and capacity of the samples. The results showed that native starch nanoparticles could be used to prepare promising nanocarriers for the controlled release of curcumin.

Keywords: starch nanoparticle, nanoprecipitation, curcumin, biomedical applications

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Authors: Pradthana Sianglam, Wittaya Ngeontae

Abstract:

A new approach for the fabrication of cadmium ion (Cd2+) sensor is demonstrated. The detection principle is based on the in-situ generation of cadmium sulfide quantum dots (CdS QDs) in the presence of chiral thiol containing compound and detection by the circular dichroism spectroscopy (CD). Basically, the generation of CdS QDs can be done in the presence of Cd2+, sulfide ion and suitable capping compounds. In addition, the strong CD signal can be recorded if the generated QDs possess chiral property (from chiral capping molecule). Thus, the degree of CD signal change depends on the number of the generated CdS QDs which can be related to the concentration of Cd2+ (excess of other components). In this work, we use the mixture of cysteamine (Cys) and L-Penicillamine (LPA) as the capping molecules. The strong CD signal can be observed when the solution contains sodium sulfide, Cys, LPA, and Cd2+. Moreover, the CD signal is linearly related to the concentration of Cd2+. This approach shows excellence selectivity towards the detection of Cd2+ when comparing to other cation. The proposed CD sensor provides low limit detection limits around 70 µM and can be used with real water samples with satisfactory results.

Keywords: circular dichroism sensor, quantum dots, enaniomer, in-situ generation, chemical sensor, heavy metal ion

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Authors: Tarun Jain, Lovnish Gupta, Soumen Basu

Abstract:

Organic pollutants like phenols and organic dyes present in industrial waste water are posing a hazardous threat to aquatic ecosystem. Several measures have been adopted for the neutralization and photodecomposition of these harmful organic moieties, among these semiconductor photocatalysis has been provided a major thrust after the discovery of Honda-Fujishema effect. Present study demonstrates the adsorption of TiO2- P25 in nano size (~36 nm) on cement balls for effective photodegradation of Alizarin and penta chlorophenol (PCP) under UV light illumination. Triton-X was used as a stabilizer for effective adsorption of TiO2 on cement balls (TCB) followed by calcination at ~300oC for 4 h. The TCB’s were dispersed randomly in a self designed reactor for phototcatalytic performance as shown in scheme 1. The change in concentration of alizarin and PCP was observed under UV-Vis spectroscopy, PCP was detoxified within 40 min while alizarin photodecomposed within 15 min of UV light irradiation. Taking into consideration the go green slogan and future prospective this technique can be also utilized under visible light and on mass scale because this is an effective tool for environmental remediation and waste water treatment.

Keywords: organic pollutants, TiO2 cement balls, photodegradation, UV light irradiation

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Authors: Imen Harabi, Hanae Toura, Safa Jemai, Bernabe Mari Soucase

Abstract:

A promising alternative to traditional Quantum Dots QD materials, which contain toxic heavy elements such as lead and cadmium, sheds light on indium phosphide quantum dots (InP QDs) Owing to improve the quantum yields of photoluminescence and other properties. InP, InP/ZnS core/shell and InP/ZnS/ZnS core/shell/shell Quantum Dots (QDs) were synthetized by the hot injection method. The optical and structural properties of the core InP QDs, InP/ZnS QDs, and InP/ZnS/ZnS QDs have being considered by several techniques such as X-ray diffraction, transmission electron microscopy, optical spectroscopy, and photoluminescence. The average diameter of InP, InP/ZnS, and InP/ZnS/ZnS Quantum Dots (QDs) was varying between 10 nm, 5.4 nm, and 4.10 nm. This experience revealed that the surface morphology of the Quantum Dots has a more regular spherical form with color variation of the QDs in solution. The emission peak of colloidal InP Quantum Dots was around 530 nm, while in InP/ZnS, the emission peak is displayed and located at 598 nm. whilst for InP/ZnS/ZnS is placed at 610 nm. Furthermore, an enhanced PL emission due to a passivation effect in the ZnS-covered InP QDs was obtained. Add the XRD information FWHM of the principal peak of InP QDs was 63 nm, while for InP/ZnS was 41 nm and InP/ZnS/ZnS was 33 nm. The effect of the Zinc stearate precursor concentration on the optical, structural, surface chemical of InP and InP/ZnS and InP/ZnS/ZnS QDs will be discussed.

Keywords: indium phosphide, quantum dot, nanoparticle, core-shell, multishell, luminescence

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Authors: Mohamed Deyab

Abstract:

The global lubricant additives market size was USD 14.35 billion in 2015. The industry is characterized by increasing additive usage in base oil blending for longer service life and performance. These additives improve the viscosity of oil, act as detergents, defoamers, antioxidants, and antiwear agents. Since additives play a significant role in base oil blending and subsequent formulations as they are critical materials in improving specification and performance of oils. Herein, we report on the synthesis and characterization of three imidazolium derivatives and their application as antioxidants, detergents and antiwear agents. The molecular structure and characterizations of these ionic liquids were confirmed by elemental analysis, FTIR, X-Ray Diffraction (XRD) and 1HNMR spectroscopy. Thermo gravimetric analysis (TGA), is used to study the degradation and thermal stability of the studied base stock samples. It was found that all the prepared ionic liquids additives have excellent power of dispersion and detergency. The ionic liquids as additives to engine oil reduced the friction (38%) and wear volume (76%) of steel balls. The obtained results show that the ionic liquids have an oxidation inhibitor up to 95%.

Keywords: reused lubricating oil, waste, petroleum, ionic liquids

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Authors: Ahmad N. Abu-Baker

Abstract:

This study investigated the corrosion of a group of heritage silver-copper alloy coins and their conservation treatment by potentiostatic methods. The corrosion products of the coins were characterized by a combination of scanning electron microscopy/ energy-dispersive X-ray spectroscopy (SEM/EDX) and X-ray diffraction (XRD) analyses. Cathodic polarization curves, measured by linear sweep voltammetry (LSV), also identified the corrosion products and the working conditions to treat the coins using a potentiostatic reduction method, which was monitored by chronoamperometry. The corrosion products showed that the decay mechanisms were dominated by selective attack on the copper-rich phases of the silver-copper alloys, which is consistent with an internal galvanic corrosion phenomenon, which leads to the deposition of copper corrosion products on the surface of the coins. Silver chloride was also detected on the coins, which reflects selective corrosion of the silver-rich phases under different chemical environments. The potentiostatic treatment showed excellent effectiveness in determining treatment parameters and monitoring the reduction process of the corrosion products on the coins, which helped to preserve surface details in the cleaning process and to prevent over-treatment.

Keywords: silver alloys, corrosion, conservation, heritage

Procedia PDF Downloads 140