Search results for: hydroxyl complexes

Authors: D. Artamonov, A. Tsibulnikova, I. Samusev, V. Bryukhanov, A. Kozhevnikov

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The synthesis and luminescent properties of Yb₂O₃, Nd₂O₃@Bi₂O₃ complex with upconversion generation are discussed in this work. The obtained samples were measured in the visible region of the spectrum under excitation with a wavelength of 980 nm. The studies showed that the obtained complexes have a high degree of stability and intense luminescence in the wavelength range of 400-750 nm. Consideration of the time dependence of the intensity of the upconversion luminescence allowed us to conclude that the enhancement of the intensity occurs in the time interval from 5 to 30 min, followed by the appearance of a stationary mode.

Keywords: lasers, luminescence, upconversion photonics, rare earth metals

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Authors: Asmaa M. Fahim

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In this investigation, the (E)-2-cyano-3-(dimethylamino)-N-(2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl)acrylam-ide (4) which used TAM as a template which interacts with Methacrylic Acid (MAA) monomer, in the presence of CH₃CN as progen. The TAM-MMA complex interactions are dependent on stable hydrogen bonding interaction between the carboxylic acid group of TAM(Template) and the hydroxyl group of MMA(methyl methacrylate) with minimal interference of porogen CH₃CN. The physical computational studies were used to optimize their structures and frequency calculations. The binding energies between TAM with different monomers showed the most stable molar ratio of 1:4, which was confirmed through experimental analysis. The optimized polymers were investigated in industrial applications.

Keywords: molecular imprinted polymer, computational studies, SEM, spectral analysis, industrial applications

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Authors: Juliana A. B. Silva, Caio H. T. L. Albuquerque, Leonardo L. dos Santos, Cristiane K. Oliveira, Ivani Malvestiti, Fernando Hallwass, Ricardo L. Longo

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Complexes with lanthanide ions have been extensively studied due to their applications as luminescent, magnetic and catalytic materials as molecular or extended crystals, thin films, glasses, polymeric matrices, ionic liquids, and in solution. NMR chemical shift data in solution have been reported and suggest fluxional structures in a wide range of coordination compounds with rare earth ions. However, the fluxional mechanisms for these compounds are still not established. This structural fluxionality may affect the photophysical, catalytic and magnetic properties in solution. Thus, understanding the structural interconversion mechanisms may aid the design of coordination compounds with, for instance, improved (electro)luminescence, catalytic and magnetic behaviors. The [Eu(btfa)₃bipy] complex, where btfa= 4,4,4-trifluoro-1-phenyl-1,3-butanedionate and bipy= 2,2’-bipiridyl, has a well-defined X-ray crystallographic structure and preliminary 1H NMR data suggested a structural fluxionality. Thus, we have investigated a series of coordination compounds with lanthanide ions [Ln(btfa)₃L], where Ln = La, Eu, Gd or Yb and L= bipy or phen (phen=1,10-phenanthroline) using a combined theoretical-experimental approach. These complexes were synthesized and fully characterized, and detailed NMR measurements were obtained. They were also studied by quantum chemical computational methods (DFT-PBE0). The aim was to determine the relevant factors in the structure of these compounds that favor or not the fluxional behavior. Measurements of the 1H NMR signals at variable temperature in CD₂Cl₂ of the [Eu(btfa)₃L] complexes suggest that these compounds have a fluxional structure, because the crystal structure has non-equivalent btfa ligands that should lead to non-equivalent hydrogen atoms and thus to more signals in the NMR spectra than those obtained at room temperature, where all hydrogen atoms of the btfa ligands are equivalent, and phen ligand has an effective vertical symmetry plane. For the [Eu(btfa)₃bipy] complex, the broadening of the signals at –70°C provides a lower bound for the coalescence temperature, which indicates the energy barriers involved in the structural interconversion mechanisms are quite small. These barriers and, consequently, the coalescence temperature are dependent upon the radii of the lanthanide ion as well as to their paramagnetic effects. The PBE0 calculated structures are in very good agreement with the crystallographic data and, for the [Eu(btfa)₃bipy] complex, this method provided several distinct structures with almost the same energy. However, the energy barrier for structural interconversion via dissociative pathways were found to be quite high and could not explain the experimental observations. Whereas the pseudo-rotation pathways, involving the btfa and bipy ligands, have very small activation barriers, in excellent agreement with the NMR data. The results also showed an increase in the activation barrier along the lanthanide series due to the decrease of the ionic radii and consequent increase of the steric effects. TD-DFT calculations showed a dependence of the ligand donor state energy with different structures of the complex [Eu(btfa)₃phen], which can affect the energy transfer rates and the luminescence. The energy required to promote the structural fluxionality may also enhance the luminescence quenching in solution. These results can aid in the design of more luminescent compounds and more efficient devices.

Keywords: computational chemistry, lanthanide-based compounds, NMR, structural fluxionality

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Authors: Ammar Z. Alshemary, Yi-Fan Goh, Rafaqat Hussain

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Magnesium (Mg2+), strontium (Sr2+) and sulphate ions (SO42-) were successfully substituted into hydroxyapatite (Ca10-x-y MgxSry(PO4)6-z(SO4)zOH2-z) structure through ion exchange process at cationic and anionic sites. Mg2+and Sr2+ ions concentrations were varied between (0.00-0.10), keeping concentration of SO42- ions at z=0.05. [Mg (NO3)2], [Sr (NO3)2] and (Na2SO4) were used as Mg2+, Sr2+, and SO42- sources respectively. The synthesized white precipitate were subjected to heat treatment at 500ºC and finally characterized by X-ray diffraction (XRD) and Fourier Transform infra-red spectroscopy (FTIR). The results showed that the substitution of Mg2+, Sr2+ and SO42- ions into the HA lattice resulted in an increase in the broadness and reduction of XRD peaks. This confirmed that the crystallinity was reduced due to the substitution of ions. Similarly, FTIR result showed the effect of substitution on phosphate bands as well as exchange of hydroxyl group by SO42- ions to balance the charges on HA surface.

Keywords: hydroxyapatite, substitution, characterization, XRD, FTIR

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Authors: Fanny Desbiolles, Laure Malleret, Isabelle Laffont-Schwob, Christophe Tiliacos, Anne Piram, Mohamed Sarakha, Pascal Wong-Wah-Chung

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Pharmaceuticals in the environment have become a very hot topic in the recent years. This interest is related to the large amounts dispensed and to their release in urine or faeces from treated patients, resulting in their ubiquitous presence in water resources and wastewater treatment plants (WWTP) effluents. Thereby, many studies focused on the prediction of pharmaceuticals’ behaviour, to assess their fate and impacts in the environment. Carbamazepine is a widely consumed psychotropic pharmaceutical, thus being one of the most commonly detected drugs in the environment. This organic pollutant was proved to be persistent, especially with respect to its non-biodegradability, rendering it recalcitrant to usual biological treatment processes. Consequently, carbamazepine is very little removed in WWTP with a maximum abatement rate of 5 % and is then often released in natural surface waters. To better assess the environmental fate of carbamazepine in aqueous media, its photochemical transformation was undertaken in four natural waters (two French rivers, the Berre salt lagoon, Mediterranean Sea water) representative of coastal and inland water types. Kinetic experiments were performed in the presence of light using simulated solar irradiation (Xe lamp 300W). Formation of short-lifetime species was highlighted using chemical trap and laser flash photolysis (nanosecond). Identification of transformation by-products was assessed by LC-QToF-MS analyses. Carbamazepine degradation was observed after a four-day exposure and an abatement of 20% maximum was measured yielding to the formation of many by-products. Moreover, the formation of hydroxyl radicals (•OH) was evidenced in waters using terephthalic acid as a probe, considering the photochemical instability of its specific hydroxylated derivative. Correlations were implemented using carbamazepine degradation rate, estimated hydroxyl radical formation and chemical contents of waters. In addition, laser flash photolysis studies confirmed •OH formation and allowed to evidence other reactive species, such as chloride (Cl2•-)/bromine (Br2•-) and carbonate (CO3•-) radicals in natural waters. Radicals mainly originate from dissolved phase and their occurrence and abundance depend on the type of water. Rate constants between reactive species and carbamazepine were determined by laser flash photolysis and competitive reactions experiments. Moreover, LC-QToF-MS analyses of by-products help us to propose mechanistic pathways. The results will bring insights to the fate of carbamazepine in various water types and could help to evaluate more precisely potential ecotoxicological effects.

Keywords: carbamazepine, kinetic and mechanistic approaches, natural waters, photodegradation

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Authors: Kai-Cheng Yang, Yen-Ling Chen, Er-Chieh Cho, Kuen-Chan Lee

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Titanium dioxide nanomaterials offer superior protection for human skin against the full spectrum of ultraviolet light. However, some literature reviews indicated that it might be associated with adverse effects such as cytotoxicity or reactive oxygen species (ROS) due to their nanoscale. The surface of fullerene is covered with π electrons constituting aromatic structures, which can effectively scavenge large amount of radicals. Unfortunately, fullerenes are poor solubility in water, severe aggregation, and toxicity in biological applications when dispersed in solvent have imposed the limitations to the use of fullerenes. Carboxyfullerene acts as the scavenger of radicals for several years. Some reports indicate that carboxyfullerene not only decrease the concentration of free radicals in ambience but also prevent cells from reducing the number or apoptosis under UV irradiation. The aim of this study is to decorate fullerene –C70-carboxylic acid (C70-COOH) on the surface of titanium dioxide nanoparticles (P25) for the purpose of scavenging ROS during the irradiation. The modified material is prepared through the esterification of C70-COOH with P25 (P25/C70-COOH). The binding edge and structure are studied by using Transmission electron microscope (TEM) and Fourier transform infrared (FTIR). The diameter of P25 is about 30 nm and C70-COOH is found to be conjugated on the edge of P25 in aggregation morphology with the size of ca. 100 nm. In the next step, the FTIR was used to confirm the binding structure between P25 and C70-COOH. There are two new peaks are shown at 1427 and 1720 cm-1 for P25/C70-COOH, resulting from the C–C stretch and C=O stretch formed during esterification with dilute sulfuric acid. The IR results further confirm the chemically bonded interaction between C70-COOH and P25. In order to provide the evidence of scavenging radical ability of P25/C70-COOH, we chose pyridoxine (Vit.B6) and terephthalic acid (TA) to react with singlet oxygen and hydroxyl radicals. We utilized these chemicals to observe the radicals scavenging statement via detecting the intensity of ultraviolet adsorption or fluorescence emission. The UV spectra are measured by using different concentration of C70-COOH modified P25 with 1mM pyridoxine under UV irradiation for various duration times. The results revealed that the concentration of pyridoxine was increased when cooperating with P25/C70-COOH after three hours as compared with control (only P25). It indicates fewer radicals could be reacted with pyridoxine because of the absorption via P25/C70-COOH. The fluorescence spectra are observed by measuring P25/C70-COOH with 1mM terephthalic acid under UV irradiation for various duration times. The fluorescence intensity of TAOH was decreased in ten minutes when cooperating with P25/C70-COOH. Here, it was found that the fluorescence intensity was increased after thirty minutes, which could be attributed to the saturation of C70-COOH in the absorption of radicals. However, the results showed that the modified P25/C70-COOH could reduce the radicals in the environment. Therefore, we expect that P25/C70-COOH is a potential materials in using for antioxidant.

Keywords: titanium dioxide, fullerene, radical scavenging activity, antioxidant

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Authors: S. Raeis Farshid, B. Raeis Farshid

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Ag-TiO₂ nanocomposites were prepared by the sol-gel method with and without additives such as carboxy methyl cellulose (CMC), polyethylene glycol (PEG), polyvinyl pyrrolidone (PVP), and hydroxyl propyl cellulose (HPC). The characteristics of the prepared Ag-TiO₂ nanocomposites were identified by Fourier Transform Infra-Red spectroscopy (FTIR), X-Ray Diffraction (XRD), and scanning electron microscopy (SEM) methods. The additives have a significant effect on the particle size distribution and photocatalytic activity of Ag-TiO₂ nanocomposites. SEM images have shown that the particle size distribution of Ag-TiO₂ nanocomposite in the presence of HPC was the best in comparison to the other samples. The photocatalytic activity of the synthesized nanocomposites was investigated for decolorization of methyl orange (MO) in water under UV-irradiation in a batch reactor, and the results showed that the photocatalytic activity of the nanocomposites had been increased by CMC, PEG, PVP, and HPC, respectively.

Keywords: sol-gel method, Ag-TiO₂, decolorization, photocatalyst, nanocomposite

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Authors: A. Bara, D. Barkat

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Liquid-liquid extraction is one of the most useful techniques for selective removal and recovery of metal ions from aqueous solutions, applied in purification processes in numerous chemical and metallurgical industries. In this work, The liquid-liquid extraction of cobalt (II) and copper (II) from aqueous solution by capric acid (HL) in chloroform at 25°C has been studied. Our interest in this paper is to study the effect of concentration of capric acid on the extraction of Co(II) and Cu(II) to see the complexes could be formed in the organic phase using various concentration of capric acid. The extraction of cobalt (II) and copper (II) is extracted as the complex CoL2 (HL )2, CuL2 (HL)2.

Keywords: capric acid, Cobalt(II), copper(II), liquid-liquid extraction

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Authors: Iwona Misztalewska-Turkowicz, Agnieszka Z. Wilczewska, Karolina H. Markiewicz

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Carbenes - species which possess neutral carbon atom with two shared and two unshared valence electrons, are known for their high reactivity and instability. Nevertheless, it is also known, that some carbenes i.e. N-heterocyclic carbenes (NHCs), can form stable crystals. The usability of NHCs in organic synthesis was studied. Due to their exceptional properties (high nucleophilicity) NHCs are commonly used as organocatalysts and also as ligands in transition metal complexes. NHC ligands possess better electron-donating properties than phosphines. Moreover, they exhibit lower toxicity. Due to these features, phosphines are frequently replaced by NHC ligands. In this research is discussed the synthesis of five-membered NHCs which are mainly obtained by deprotonation of azolium salts, e.g., imidazolium or imidazolinium salts. Some of them are immobilized on a solid support what leads to formation of heterogeneous, recyclable catalysts. Magnetic nanoparticles (MNPs) are often used as a solid support for catalysts. MNPs can be easily separated from the reaction mixture using an external magnetic field. Due to their low size and high surface to volume ratio, they are a good choice for immobilization of catalysts. Herein is presented synthesis of N-heterocyclic carbene copper complexes directly on the surface of magnetic nanoparticles. Formation of four different catalysts is discussed. They vary in copper oxidation state (Cu(I) and Cu(II)) and structure of NHC ligand. Catalysts were tested in Huisgen reaction, a type of copper catalyzed azide-alkyne cycloaddition (CuAAC) reaction. Huisgen reaction represents one of the few universal and highly efficient reactions in which 1,2,3-triazoles can be obtained. The catalytic activity of all synthesized catalysts was compared with activity of commercially available ones. Different reaction conditions (solvent, temperature, the addition of reductant) and reusability of the obtained catalysts were investigated and are discussed. The project was financially supported by National Science Centre, Poland, grant no. 2016/21/N/ST5/01316. Analyses were performed in Centre of Synthesis and Analyses BioNanoTechno of University of Bialystok. The equipment in the Centre of Synthesis and Analysis BioNanoTechno of University of Bialystok was funded by EU, as a part of the Operational Program Development of Eastern Poland 2007-2013, project: POPW.01.03.00-20-034/09-00 and POPW.01.03.00-20-004/11.

Keywords: N-heterocyclic carbenes, click reaction, magnetic nanoparticles, copper catalysts

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Authors: Tomilola J. Ajayi

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A category of nanovalves system containing the α-cyclodextrin (α-CD) ring on a stalk tethered to the pores of mesoporous silica nanoparticles (MSN) is theoretically and computationally modelled. This functions to control opening and blocking of the MSN pores for efficient targeted drug release system. Modeling of the nanovalves is based on the interaction between α-CD and the stalk (p-anisidine) in relation to pH variation. Conformational analysis was carried out prior to the formation of the inclusion complex, to find the global minimum of both neutral and protonated stalk. B3LYP/6-311G**(d, p) basis set was employed to attain all theoretically possible conformers of the stalk. Six conformers were taken into considerations, and the dihedral angle (θ) around the reference atom (N17) of the p-anisidine stalk was scanned from 0° to 360° at 5° intervals. The most stable conformer was obtained at a dihedral angle of 85.3° and was fully optimized at B3LYP/6-311G**(d, p) level of theory. The most stable conformer obtained from conformational analysis was used as the starting structure to create the inclusion complexes. 9 complexes were formed by moving the neutral guest into the α-CD cavity along the Z-axis in 1 Å stepwise while keeping the distance between dummy atom and OMe oxygen atom on the stalk restricted. The dummy atom and the carbon atoms on α-CD structure were equally restricted for orientation A (see Scheme 1). The generated structures at each step were optimized with B3LYP/6-311G**(d, p) methods to determine their energy minima. Protonation of the nitrogen atom on the stalk occurs at acidic pH, leading to unsatisfactory host-guest interaction in the nanogate; hence there is dethreading. High required interaction energy and conformational change are theoretically established to drive the release of α-CD at a certain pH. The release was found to occur between pH 5-7 which agreed with reported experimental results. In this study, we applied the theoretical model for the prediction of the experimentally observed pH-responsive nanovalves which enables blocking, and opening of mesoporous silica nanoparticles pores for targeted drug release system. Our results show that two major factors are responsible for the cargo release at acidic pH. The higher interaction energy needed for the complex/nanovalve formation to exist after protonation as well as conformational change upon protonation are driving the release due to slight pH change from 5 to 7.

Keywords: nanovalves, nanogate, mesoporous silica nanoparticles, cargo

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Authors: Sender Dovchin

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Moving beyond two main frameworks of interlingual and intralingual discrimination, this paper will address the understanding of translingual discrimination. This concept refers to discrimination based on how one uses certain languages, linguistic and communicative repertoires, which are (il)legitimised by the interactants. Translingual discrimination contributes intensity to transnational migrations processes, where migrants with transitional backgrounds seem to illustrate two main characteristics of marginalizations – “name discrimination” and “accentism”. The lifelong accumulation of these characteristics of translingual discrimination may cause negative emotionality, such as translingual inferiority complexes, to its victims. As a result, these transnational migrants seem to adopt varied coping strategies such as CV-whitening and accent purifications while probing for translingual safe spaces. The presentation concludes with the socio-cultural and pedagogical implications of translingual discrimination in relation to the language usage of transnational migrants.

Keywords: accentism, discrimination, migrants, translingualism

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Authors: Azza. A. Al-Ghamdi, Abir. A. Abdel-Naby

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The construction of Nitro -N-amino phenyl maleimide branches onto Cellulose acetate (CA) substrate by free radical graft copolymerization using benzoyl peroxide as initiator led to formation of highly thermal stable copolymers as shown from the results of gravimetric analysis (TGA). CA-g-2,4-dinitro amino phenyl maleimide exhibited higher thermal stability than the CA-g-4-nitro amino phenyl maleimide as shown from the initial decomposition temperature (T_o). This is due to the ability of nitro group to form hydrogen bonding with hydroxyl group of the glucopyranose ring which increases the crystallinity of polymeric matrix. The crystalline shapes representing the graft part are clearly distinct in the Emission scanning electron microscope (ESEM) morphology of the copolymer. A suggested reaction mechanism for the grafting process was also discussed.

Keywords: Cellulose acetate, Crystallinity, Graft copolymerization, Thermal properties

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Authors: Mohamed Nasraoui

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Spatial ore distribution, ore heterogeneity and their links with geological processes involved in Niobium concentration are all factors for consideration when bridging field observations to extraction scheme. Indeed, mineralogy changes of Nb-hosting phases, their textural relationships with hydrothermal or secondary minerals, play a key control over mineral processing. This study based both on filed work and ore characterization presents data from several Nb-deposits related to carbonatite complexes. The results obtained by a wide range of analytical techniques, including, XRD, XRF, ICP-MS, SEM, Microprobe, Spectro-CL, FTIR-DTA and Mössbauer spectroscopy, demonstrate how geometallurgical assessment, at all stage of mine development, can greatly assist in the design of a suitable extraction flowsheet and data reconciliation.

Keywords: carbonatites, Nb-geometallurgy, Nb-mineralogy, mineral processing.

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Authors: Debashis Nath

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Drawn from multiple reanalysis datasets, an increasing trend and westward shift in the number of Potential Vorticity (PV) intrusion events over the Pacific are evident. The increased frequency can be linked to a long-term trend in upper tropospheric (UT, 200 hPa) equatorial westerly wind and subtropical jets (STJ) during boreal winter to spring. These may be resulting from anomalous warming and cooling over the western Pacific warm pool and the tropical eastern Pacific, respectively. The intrusions brought dry and ozone rich air of stratospheric origin deep into the tropics. In the tropical UT, interannual ozone variability is mainly related to convection associated with El Niño/Southern Oscillation. Zonal mean stratospheric overturning circulation organizes the transport of ozone rich air poleward and downward to the high and midlatitudes leading there to higher ozone concentration. In addition to these well described mechanisms, we observe a long-term increasing trend in ozone flux over the northern hemispheric outer tropical (10–25°N) central Pacific that results from equatorward transport and downward mixing from the midlatitude UT and lower stratosphere (LS) during PV intrusions. This increase in tropospheric ozone flux over the Pacific Ocean may affect the radiative processes and changes the budget of atmospheric hydroxyl radicals. The results demonstrate a long-term increase in outer tropical Pacific PV intrusions linked with the strengthening of the upper tropospheric equatorial westerlies and weakening of the STJ. Zonal variation in SST, characterized by gradual warming in the western Pacific–warm pool and cooling in the central–eastern Pacific, is associated with the strengthening of the Pacific Walker circulation. In the Western Pacific enhanced convective activity leads to precipitation, and the latent heat released in the process strengthens the Pacific Walker circulation. However, it is linked with the trend in global mean temperature, which is related to the emerging anthropogenic greenhouse signal and negative phase of PDO. On the other hand, the central-eastern Pacific cooling trend is linked to the weakening of the central–eastern Pacific Hadley circulation. It suppresses the convective activity due to sinking air motion and imports less angular momentum to the STJ leading to a weakened STJ. While, more PV intrusions result from this weaker STJ on its equatorward side; significantly increase the stratosphere-troposphere exchange processes on the longer timescale. This plays an important role in determining the atmospheric composition, particularly of tropospheric ozone, in the northern outer tropical central Pacific. It may lead to more ozone of stratospheric origin in the LT and even in the marine boundary, which may act as harmful pollutants and affect the radiative processes by changing the global budgets of atmospheric hydroxyl radicals.

Keywords: PV intrusion, westerly duct, ozone, Central Pacific

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Authors: Akintayo Emmanuel Temitope, Akintayo Cecilia Olufunke, Ziegler Thomas

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Bio-polyols are important components in polyurethane industries. The preliminary studies into the synthesis of bio-polyol products (epoxy-polyol and epoxyl-polyurethanes) from Jatropha curcas were investigated. The reactions were followed by both infrared and nuclear magnetic resonance. Physico-chemical characterisation of the samples for iodine value (IV), acid value (AV), saponification value (SV) and hydroxyl value (HV) were carried out. Thermal transitions of the products were studied by heating 5 mg of the sample from 20ºC to 800ºC and then cooling down to -500ºC on a differential scanning calorimeter (DSC). The preparation of epoxylpolyol and polyurethane from Jatropha curcas oil was smooth and efficient. Results of film and solubility properties revealed that coatings of Jatropha curcas epoxy-polyurethanes performed better with increased loading of toluylene 2, 4-diisocyanate (TDI) up to 2 wt% while their solvent resistance decreased beyond a TDI loading of 1.2 wt%. DSC analysis shows the epoxy-polyurethane to be less stable compared to the epoxy-polyol.

Keywords: synthesis, epoxy-polyol, epoxy-polyurethane, jatropha curcas oil

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Authors: Siham Mezher Yousif, Intisar Yahiya Mohammed, Salma Nagem Mouhy

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Low Density Polyethylene is a thermoplastic resin extracted from petroleum based, whereas the wax is an oily organic component that is contains of alkanes, ester, polyester, and hydroxyl ester. The purpose of this research is to find out the optimum conditions of the wax produced by inducing with LDPE. The experiments were carried out by mixing different percentages of wax and LDPE to produce different polymer/wax compositions, in which lower values of the penetration, thickness, and electrical conductivity are obtained with increasing of mixing ratio of LDPE/wax which showed results of 19 mm penetration, 692 micron thickness and 5.9 mA electrical conductivity for 90 wt % of LDPE/wax) maximum mixing ratio (. It’s found that the optimum results regarding penetration, enamel thickness, and electrical conductivity “according to the enamel hardness, insulation properties, and economic aspects” are 20 mm, 276 micron, and 6.2 mA respectively.

Keywords: paraffin wax, low density polyethylene, blending, mixing ratio, bleaching

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Authors: Yuting Wu, Faraz Choudhury, Daniel Benjamin, James Whalin, Joshua Blatz, Leon Shohet, Michael Sussman, Mark Richards

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Plasma-Induced Modification of Biomolecules (PLIMB) has been developed as a technology, which, together with mass spectrometry, measures three-dimensional structural characteristics of proteins. This technique uses hydroxyl radicals generated by atmospheric-pressure plasma discharge to react with the solvent-accessible side chains of protein in an aqueous solution. In this work, we investigate the three-dimensional structure of hemoglobin and myoglobin using PLIMB. Additional modifications to these proteins, such as oxidation, fragmentations, and conformational changes caused by PLIMB are also explored. These results show that PLIMB, coupled with mass spectrometry, is an effective way to determine solvent access to hemoproteins. Furthermore, we show that many factors, including pH and the electrical parameters used to generate the plasma, have a significant influence on solvent accessibility.

Keywords: plasma, hemoglobin, myoglobin, solvent access

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Authors: Siti Rahmah Shamsuri, Eiichiro Matsubara, Shohei Shiomi

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The 1D nanomaterial is far surpassed the 0D nanomaterial. It does not just offer most of the benefit of the 0D nanomaterial such as the large surface area, a great number of active site and an efficient interfacial charge transfer but also can assemble into free-standing and flexible electrode due to their high aspect ratio. Thus, it is essential to develop a simple and ease synthesis of this 1D nanomaterial for the practical application. Here, nickel nanowire/cellulose hybrid has been successfully fabricated via a simple liquid-phase method with the assist of the magnetic field. A finer nickel nanowire was heterogeneously nucleated on the surface of the cellulose fiber, which demonstrated the effect of the hydroxyl group on the cellulose structure. The result of the nickel nanowire size was found to vary from 66-114 nm. A detailed discussion on the mechanism of the nickel nanowire/ cellulose hybrid formation is also shown in this paper.

Keywords: cellulose nanofiber, liquid-phase reduction, metal nanowire, nano hybrid material

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Authors: Farhat Jabeen, Muhammad Asad

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The study assessed the curative potential of Moringa olifera seeds against copper oxide nanoparticles induced toxicity in Oreochromis mossambicus. In order to investigate the curative potential of M. olifera seeds, firstly we examine its chemical composition, secondary metabolites, and bioactive compounds including hydroxyl-cinnamic acids, flavanols and hydroxybenzoic acids through standard methods and high performance liquid chromatography. In current study, the potential sub-lethal toxic dose of CuO-NPs (0.12 mg/l) was investigated through pilot experiment and three non-lethal doses (low=32, medium=48 and high=96 mg/l) of M. olifera were selected on the basis of its LC50 value for O. mossambicus. The experimental fish, O. mossambicus (n=100 of approximately 20 g each) were procured from Manawan Fisheries Complex, Lahore, and acclimatized for two weeks in glass aquaria. Experiment was conducted in accordance with the guidelines of Institutional Animal Ethics Committee, Government College University Faisalabad, Pakistan. During acclimatization and experimental period, fish received the commercial fish feed at 2.5% body weight daily. In order to assess the curative effect of M. olifera against CuO NPs induced toxicity, O. mossambicus were randomly divided into five groups and were designated as control (C) without any treatment, positive control (G*) exposed to potential toxic dose of CuO-NPs at 0.12 mg/l, and three treated groups namely G1, G2, and G3 co-treated with 0.12 mg/l of CuO-NPs plus different doses of M. olifera seed extract at 32, 48, and 96 mg/l, respectively for 56 days. Fish were exposed to waterborne CuO NPs and M. olifera seed extract. CuO-NPs treatment was ceased after 28 days but the doses of M. olifera were continued for 56 days. Blood was taken after 28 and 56 days through caudal venipuncture. Liver and intestine were taken for oxidative stress and histological studies after 56 days. In M. olifera seeds, moisture contents, crude protein, lipids, carbohydrates and ash were recorded as 3.8, 37.83, 32.52, 46.12, and 7.75%, respectively on dry weight basis. Total energy was recorded as 627.36 kcal/100g. Qualitative analysis of M. olifera seeds showed the presence of terpenoids, saponins, flavonoids, alkaloids and phenolics, while its quantitative analysis showed the considerable amount of total phenolics, flavonoids, saponins, and alkaloids as 134.75, 170.15, 1.57, and 0.4 µg/mg, respectively. Analysis of bioactive compounds in M. olifera seeds showed the presence of hydroxy-cinnamic acids (6.07 µg/ml), flavanols (71.72 µg/ml), and hydroxyl benzoic acids (97.82 µg/ml). The results showed that M. oliefera seed extract at 48 and 56 mg/l was able to cure against the toxic effects of CuO-NPs. The significant changes were observed in G* and G1 for sero-hepatic enzymes, anti-oxidants and histological profile. The investigations of this study showed that M. olifera is a good curative agent against potential induced toxicity of CuO-NPs in O. mossambicus. The curative effect of M. olifera is attributed to the presence of higher amount of secondary metabolites and bioactive compounds. This study suggested the use of M. olifera to curate different ailments in fish and other organisms.

Keywords: CuO nanoparticles, curative, Moringa olifera, Oreochromis mossambicus

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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: A. Masek, M. Zaborski

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Electrochemical oxidation of dodecyl gallate (lauryl gallate), the main monomer flavanol found in green tea, was investigated on platinum electrodes using cyclic voltammetry (CV) and differential pulse (DPV) methods. The rate constant, electron transfer coefficient and diffusion coefficients were determined for dodecyl gallate electrochemical oxidation. The oxidation mechanism proceeds in sequential steps related to the hydroxyl groups in the aromatic ring of dodecyl gallate. Confirmed antioxidant activity of lauryl gallate verified its use in polymers as an environment-friendly stabiliser to improve the resistance to aging of the elastomeric materials. Based on the energy change of the deformation, cross-linking density and time of the oxygen induction with the TG method, we confirmed the high antioxidant activity of lauryl gallate in polymers. Moreover, the research on biodegradation confirmed the environment-friendly influence of the antioxidant by increasing the susceptibility of the elastomeric materials to disintegration by mildew mushrooms.

Keywords: polymers, flavonoids, stabilization, ageing

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Authors: Diana M. Torres, Anngie K. Hernandez, Andrea Villareal, Magda R. Gomez, Sadao Kobayashi

Abstract:

Colombian Garlic crops exhibited mild mosaic, yellow stripes, and deformation. This group of symptoms suggested a viral infection. Several viruses belonging to the genera Potyvirus, Carlavirus and Allexivirus are known to infect garlic and lower their yield worldwide, but in Colombia, there are no studies of viral infections in this crop, only leek yellow stripe virus (LYSV) has been reported to our best knowledge. In Colombia, there are no management strategies for viral diseases in garlic because of the lack of information about viral infections on this crop, which is reflected in (i) high prevalence of viral related symptoms in garlic fields and (ii) high dispersal rate. For these reasons, the purpose of the present study was to evaluate the viral status of garlic in Colombia, which can represent a major threat on garlic yield and quality for this country 55 symptomatic leaf samples were collected for virus detection by RT-PCR and mechanical inoculation. Total RNA isolated from infected samples were subjected to RT-PCR with primers 1-OYDV-G/2-OYDV-G for Onion yellow dwarf virus (OYDV) (expected size 774pb), 1LYSV/2LYSV for LYSV (expected size 1000pb), SLV 7044/SLV 8004 for Shallot latent virus (SLV) (expected size 960pb), GCL-N30/GCL-C40 for Garlic common latent virus (GCLV) (expected size 481pb) and EF1F/EF1R for internal control (expected size 358pb). GCLV, SLV, and LYSV were detected in infected samples; in 95.6% of the analyzed samples was detected at least one of the viruses. GCLV and SLV were detected in single infection with low prevalence (9.3% and 7.4%, respectively). Garlic generally becomes coinfected with several types of viruses. Four viral complexes were identified: three double infection (64% of analyzed samples) and one triple infection (15%). The most frequent viral complex was SLV + GCLV infecting 48.1% of the samples. The other double complexes identified had a prevalence of 7% (GCLV + LYSV and SLV + LYSV) and 5.6% of the samples were free from these viruses. Mechanical transmission experiments were set up using leaf tissues of collected samples from infected fields, different test plants were assessed to know the host range, but it was restricted to C. quinoa, confirming the presence of detected viruses which have limited host range and were detected in C. quinoa by RT-PCR. The results of molecular and biological tests confirm the presence of SLV, LYSV, and GCLV; this is the first report of SLV and LYSV in garlic plants in Colombia, which can represent a serious threat for this crop in this country.

Keywords: SLV, GCLV, LYSV, leek yellow stripe virus, Allium sativum

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Authors: Nazila Dehbari, Javad Tavakoli, Yakani Kambu, Youhong Tang

Abstract:

Superabsorbent hydrogels (SAP), as an enviro-sensitive material have been widely used for industrial and biomedical applications due to their unique structure and capabilities. Poor mechanical properties of SAPs - which is extremely related to their large volume change – count as a great weakness in adopting for high-tech applications. Therefore, improving SAPs’ mechanical properties via toughening methods by mixing different types of cross-linked polymer or introducing energy-dissipating mechanisms is highly focused. In this work, in order to change the intrinsic brittle character of commercialized Poly Acrylic Acid (here as SAP) to be semi-ductile, a commercial available highly branched tree-like dendritic polymers with numerous –OH end groups known as hyper-branched polymer (HB) has been added to PAA-SAP system in a single step, cost effective and environment friendly solvent casting method. Samples were characterized by FTIR, SEM and TEM and their physico-chemical characterization including swelling capabilities, hydraulic permeability, surface tension and thermal properties had been performed. Toughness energy, stiffness, elongation at breaking point, viscoelastic properties and samples extensibility were mechanical properties that had been performed and characterized as a function of samples lateral cracks’ length in different HB concentration. Addition of HB to PAA-SAP significantly improved mechanical and surface properties. Increasing equilibrium swelling ratio by about 25% had been experienced by the SAP-HB samples in comparison with SAPs; however, samples swelling kinetics remained without changes as initial rate of water uptake and equilibrium time haven’t been subjected to any changes. Thermal stability analysis showed that HB is participating in hybrid network formation while improving mechanical properties. Samples characterization by TEM showed that, the aggregated HB polymer binders into nano-spheres with diameter in range of 10–200 nm. So well dispersion in the SAP matrix occurred as it was predictable due to the hydrophilic character of the numerous hydroxyl groups at the end of HB which enhance the compatibility of HB with PAA-SAP. As the profused -OH groups in HB could react with -COOH groups in the PAA-SAP during the curing process, the formation of a 2D structure in the SAP-HB could be attributed to the strong interfacial adhesion between HB and the PAA-SAP matrix which hinders the activity of PAA chains (SEM analysis). FTIR spectra introduced new peaks at 1041 and 1121 cm-1 that attributed to the C–O(–OH) stretching hydroxyl and O–C stretching ester groups of HB polymer binder indicating the incorporation of HB polymer into the SAP structure. SAP-HB polymer has significant effects on the final mechanical properties. The brittleness of PAA hydrogels are decreased by introducing HB as the fracture energies of hydrogels increased from 8.67 to 26.67. PAA-HBs’ stretch ability enhanced about 10 folds while reduced as a function of different notches depth.

Keywords: superabsorbent polymer, toughening, viscoelastic properties, hydrogel network

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Authors: Debajit Kalita, Macmillan Nongkhlaw, S. R. Joshi

Abstract:

Mercury (Hg) is a highly toxic heavy metal released both from naturally occurring volcanoes and anthropogenic activities like alkali and mining industries as well as biomedical wastes. Exposure to mercury is known to affect the nervous, gastrointestinal and renal systems. In the present study, a bacterial isolate identified using 16S rRNA marker as Paenibacillus jamilae PKR1 isolated from India’s largest sandstone-type uranium deposits, containing an average of 0.1% U3O8, was found to be resistance to Hg contamination under culture conditions. It showed strong hydrophobicity as revealed by SAT, MATH, PAT, SAA adherence assays. The Fourier Transform Infrared (FTIR) spectra showed the presence of hydroxyl, amino and carboxylic functional groups on the cell surface EPS which are known to contribute in the binding of metals. It is proposed that the characterized isolate tolerating up to 4.0mM of mercury provides scope for its application in bioremediation of mercury from contaminated sites.

Keywords: mercury, Domiasiat, uranium, paenibacillus jamilae, hydrophobicity, FTIR

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Authors: A. Loayza

Abstract:

Wood acetilationhapens when woody cell wall is saturated with acetic anhydride, the free hydroxyl groups present on cellulosic structures are replaced. Thus, the capillary spaces are filled with acetyl groups, and this replacement avoids further reactions with water. But, there is no information about wood acetilation in peruvianamzonic Wood species (SchizolobiumExcelsumVoge and CalycophyllumSpruceanum). So, in this research, we test acetylation of this two peruvian species in order to assess its ability as a protection estrategy, like the artificially cultivated species common for this type of treatment. A know experimental methodology was applied, using a laboratory reactor, evaluating the time as a principal variable. In this research, we were able to evaluate weight gains. The acetylation was carriet out considering one immersion time of 3 and 6 hours on acetic anhydride, were could it be observed weight gains ranged between 14 and 20% and the improvement of mention properties such as: a) Dimensional stability and water absorption capacity improved as well as its compressive strength.

Keywords: acetylation, calycophyllum spruceanum benth. Hook. F., cedrelinga cateniformis, copaifera langsdorffii, dimensional stability, schizolobium parahybum

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Authors: M. Das, B. P. Sarma, G. Ahmed

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Human diet can be a major source of antioxidants. Poly¬phenols, which are organic compounds present in the regular human diet, have good antioxidant property. Most of the diseases are detected too late and that cause irre¬versible damage to the body. Therefore food that forms the natural source of antioxidants can prevent free radi¬cals from damaging our body tissues. Dillenia indica and Garcinia penducalata are two major fruits, easily available in Assam, North eastern Indian state. In the present study, the in vitro antioxi¬dant properties of the fruits of these plants are compared as the decoction of these fruits form a major part of Assamese cuisine. DPPH free radical scavenging activity of the methanol, petroleum ether and water extracts of G. penducalata and D. indica fruits were carried out by the methods of Cotelle A et al. (1996). Different concentrations ranging from 10–110 ug/ml of the extracts were added to 100 uM of DPPH (2,2, Diphenyl-2-picryl hydrazyl) and the absor¬bance was read at 517 nm after incubation. Ascorbic acid was used as the standard. Different concentrations of the methanol, petroleum ether and water extracts of G. penducalata and D. indica fruits were mixed with sodium nitroprusside and incubated. Griess reagent was added to the mixtures and their optical density was read at 546 nm following the method of Marcocci et al. (1994). Ascorbic acid was used as the standard. In order to find the scavenging activity of the extracts against hydroxyl radicals, the method of Kunchandy & Ohkawa (1990) was followed.The superoxide scavenging activity of the methanol, petroleum ether and water extracts of the fruits was deter¬mined by the method of Robak & Gryglewski (1998).Six replicates were maintained in each of the experiments and their SEM was evaluated based on which, non linear regres¬sion (curve fit), exponential growth were derived to calculate the IC50 values of the SAWE and standard compounds. All the statistical analyses were done by using paired t test. The hydroxyl radical scavenging activity of the various extracts of D. indica exhibited IC50 values < 110 ug/ml concentration, the scavenging activity of the extracts of G. penducalata was surprisingly>110 ug/ml.Similarly the oxygen free radical scavenging activity of the different extracts of D. indica exhibited an IC50 value of <110 ug/ml but the methanolic extract of the same exhib¬ited a better free radical scavenging activity compared to that of vitamin C. The methanolic extract of D. indica exhibited an IC50 value better than that of vitamin C. The DPPH scavenging activities of the various extracts of D. indica and G. penducalata were <110 ug/ml but the methanolic extract of D. indica exhibited an IC50 value bet¬ter than that of vitaminc C.The higher amounts of phenolic content in the methanolic extract of D. indica might be one of the major causes for its enhanced in vitro antioxidant activity.The present study concludes that Dillenia indica and Garcinia penducalata both possesses anti oxidant activi¬ties. The anti oxidant activity of Dillenia indica is superior to that of Garcinia penducalata due to its higher phenolic content

Keywords: antioxidants, free radicals, phenolic, scavenging

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Authors: H. D. Duong, J. I. Rhee

Abstract:

In this work, gold nanoparticles in star shape (called gold nanostars, GNS) were synthesized and coated by N-(3-aminopropyl) methacrylamide hydrochloride (PA) and mercaptopropionic acid (MPA) for functionalizing their surface by amine and carboxyl groups and then investigated for ROS production. The GNS with big size and multi-tips seem to be superior in singlet oxygen production as compared with that of small GNS and less tips. However, the functioned GNS in small size could also enhance efficiency of singlet oxygen production about double as compared with that of the intact GNS. In combination with methylene blue (MB+), the functioned GNS could enhance the singlet oxygen production of MB+ after 1h of LED750 irradiation and no difference between small size and big size in this reaction was observed. In combination with 5-aminolevulinic acid (ALA), only GNS coated PA could enhance the singlet oxygen production of ALA and the small size of GNS coated PA was a little higher effect than that of the bigger size. However, GNS coated MPA with small size had strong effect on hydroxyl radical production of ALA.

Keywords: 5-aminolevulinic acid, gold nanostars, methylene blue, ROS production

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Authors: Yalçın Kılıç, İbrahim Kani

Abstract:

In recent years, interest in the synthesis of coordination compounds has greatly increased due to various application areas (such as catalysis, gas storage, luminescence). Dicarboxylic acids are often used in the synthesis of metal complexes. Bis-thiosalicylate derivative ligands contribute to the synthesis of structures of crystal engineering interest, as they can have both rigid and flexible properties. In addition, these ligands have great potential in terms of catalytic applications with the sulfur and oxygen donor atoms in their structures. In this study, we synthesized a Cu(II) complex [Cu(tsaxyl)(phen)2]•CH3OH (where tsaxyl = 2,2'-(1,2-phylenebis(methylene))bis(sulfanedyl)dibenzoate, phen = 1,10-phenantroline) and characterized through X-ray crystallography. The catalytic activities of Cu(II) complex on oxidation of ethylbenzene, cyclohexane, diphenylmethane, p-xylene were performed in acetonitrile with t-BuOOH as the source of oxygen.

Keywords: complex, crystallography, catalysis, oxidation

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Authors: María José Carrero, Ana M. Borreguero, Juan F. Rodríguez, María M. Velencoso, Ángel Serrano, María Jesús Ramos

Abstract:

Flame-retardants are incorporated in different materials in order to reduce the risk of fire, either by providing increased resistance to ignition, or by acting to slow down combustion and thereby delay the spread of flames. In this work, polyether polyols with fire retardant properties were synthesized due to their wide application in the polyurethanes formulation. The combustion of polyurethanes is primarily dependent on the thermal properties of the polymer, the presence of impurities and formulation residue in the polymer as well as the supply of oxygen. There are many types of flame retardants, most of them are phosphorous compounds of different nature and functionality. The addition of these compounds is the most common method for the incorporation of flame retardant properties. The employment of glycerol phosphate sodium salt as initiator for the polyol synthesis allows obtaining polyols with phosphate groups in their structure. However, some of the critical points of the use of glycerol phosphate salt are: the lower reactivity of the salt and the necessity of a solvent (dimethyl sulfoxide, DMSO). Thus, the main aim in the present work was to determine the amount of the solvent needed to get a good solubility of the initiator salt. Although the anionic polymerization mechanism of polyether formation is well known, it seems convenient to clarify the role that DMSO plays at the starting point of the polymerization process. Regarding the fact that the catalyst deprotonizes the hydroxyl groups of the initiator and as a result of this, two water molecules and glycerol phosphate alkoxide are formed. This alkoxide, together with DMSO, has to form a homogeneous mixture where the initiator (solid) and the propylene oxide (PO) are soluble enough to mutually interact. The addition rate of PO increased when the solvent/initiator ratios studied were increased, observing that it also made the initiation step shorter. Furthermore, the molecular weight of the polyol decreased when higher solvent/initiator ratios were used, what revealed that more amount of salt was activated, initiating more chains of lower length but allowing to react more phosphate molecules and to increase the percentage of phosphorous in the final polyol. However, the final phosphorous content was lower than the theoretical one because only a percentage of salt was activated. On the other hand, glycerol phosphate disodium salt was still partially insoluble in DMSO studied proportions, thus, the recovery and reuse of this part of the salt for the synthesis of new flame retardant polyols was evaluated. In the recovered salt case, the rate of addition of PO remained the same than in the commercial salt but a shorter induction period was observed, this is because the recovered salt presents a higher amount of deprotonated hydroxyl groups. Besides, according to molecular weight, polydispersity index, FT-IR spectrum and thermal stability, there were no differences between both synthesized polyols. Thus, it is possible to use the recovered glycerol phosphate disodium salt in the same way that the commercial one.

Keywords: DMSO, fire retardants, glycerol phosphate disodium salt, recovered initiator, solvent

Procedia PDF Downloads 248

Authors: Arzu Javadova

Abstract:

The complex of sedimentary deposits that make up the West Turkmen Basin is almost completely hidden under the Quaternary formations. The most ancient deposits emerging on the surface in some places are the deposits of the Red Color Suite of the Pliocene. Miocene deposits are exposed only at the Western end of the Kopet Dag. The main object of stratigraphic, including micropaleontological studies, were the deposits of the Quaternary and Pliocene forming marine and coastal structures. The identified stratigraphic units have certain characteristic Ostracod complexes. The fauna of the Ostracod acquires special significance in the stratification of Neogene and Quaternary deposits. Ostracods of the Neogene, Pliocene and Quaternary deposits of the West Turkmen depression are represented by a large part of the species common in the corresponding deposits of Azerbaijan and Iran.

Keywords: neogene, quaternary, turkmenistan, south caspian basin, ostracoda, foraminifera, biostratigraphy, paleontology

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