World Academy of Science, Engineering and Technology

Authors: Rabih Al-Kaysi

Abstract:

When quasi-stable solutions of 9-methylanthracene (pi-electron donor, 0.0005 M) and 1,2,4,5-Tetracyanobenzene (pi-electron acceptor, 0.0005 M) in aqueous sodium dodecyl sulfate (SDS, 0.025 M) were gently mixed, uniform-shaped rectangular charge-transfer nanocrystals precipitated out. These red colored charge-transfer (CT) crystals were composed of a 1:1-mole ratio of acceptor/ donor and are highly insoluble in water/SDS solution. The rectangular crystals morphology is semi hollow with symmetrical twin pockets reminiscent of nanocapsules. For a typical crop of nanocapsules, the dimensions are 21 x 6 x 0.5 microns with an approximate hollow volume of 1.5 x 105 nm3. By varying the concentration of aqueous SDS, mixing duration and incubation temperature, we can control the size and volume of the nanocapsules. The initial number of CT seed nanoparticles, formed by mixing the D and A solutions, determined the number and dimensions of the obtained nanocapsules formed after several hours of incubation under still conditions. Prolonged mixing of the donor and acceptor solutions resulted in plenty of initial seeds hence smaller nanocapsules. Short mixing times yields less seed formation and larger micron-sized capsules. The addition of Doxorubicin in situ with the quasi-stable solutions while mixing leads to the formation of CT nanocapsules with Doxorubicin sealed inside. The Doxorubicin can be liberated from the nanocapsules by cracking them using ultrasonication. This method can be extended to other binary CT complex crystals as well.

Keywords: charge-transfer, nanocapsules, nanocrystals, doxorubicin

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Authors: Khadijat Olabisi Abdulwahab, Mohammad Azad Malik, Paul O'Brien, Grigore Timco, Floriana Tuna

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The synthesis of spinel ferrite nanoparticles with a narrow size distribution is very crucial in their numerous applications including information storage, hyperthermia treatment, drug delivery, contrast agent in magnetic resonance imaging, catalysis, sensors, and environmental remediation. Ferrites have the general formula MFe₂O₄ (M = Fe, Co, Mn, Ni, Zn e.t.c) and possess remarkable electrical and magnetic properties which depend on the cations, method of preparation, size and their site occupancies. To the best of our knowledge, there are no reports on the use of a single source precursor to synthesise quaternary ferrite nanoparticles. Here in, we demonstrated the use of trimetallic iron pivalate cluster [CrCoFeO(O₂CᵗBu)₆(HO₂CᵗBu)₃] as a single source precursor to synthesise monodisperse cobalt chromium ferrite (FeCoCrO₄) nanoparticles by the hot injection thermolysis method. The precursor was thermolysed in oleylamine, oleic acid, with diphenyl ether as solvent at 260 °C. The effect of reaction time on the stoichiometry, phases or morphology of the nanoparticles was studied. The p-XRD patterns of the nanoparticles obtained after one hour was pure phase of cubic iron cobalt chromium ferrite (FeCoCrO₄). TEM showed that a more monodispersed spherical ferrite nanoparticles were obtained after one hour. Magnetic measurements revealed that the ferrite particles are superparamagnetic at room temperature. The nanoparticles were characterised by Powder X-ray Diffraction (p-XRD), Transmission Electron Microscopy (TEM), Energy Dispersive Spectroscopy (EDS) and Super Conducting Quantum Interference Device (SQUID).

Keywords: cobalt chromium ferrite, colloidal, hot injection thermolysis, monodisperse, reaction time, single source precursor, quaternary ferrite nanoparticles

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Authors: Gülşen Akın Evingür, Önder Pekcan

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The fractal analysis is a bridge between the microstructure and macroscopic properties of gels. Fractal structure is usually provided to define the complexity of crosslinked molecules. The complexity in gel systems is described by the fractal dimension (Df). In this study, polyacrylamide- graphene oxide (GO) composite gels were prepared by free radical crosslinking copolymerization. The fractal analysis of polyacrylamide- graphene oxide (GO) composite gels were analyzed in various GO contents during gelation and were investigated by using Fluorescence Technique. The analysis was applied to estimate Df s of the composite gels. Fractal dimension of the polymer composite gels were estimated based on the power law exponent values using scaling models. In addition, here we aimed to present the geometrical distribution of GO during gelation. And we observed that as gelation proceeded GO plates first organized themselves into 3D percolation cluster with Df=2.52, then goes to diffusion limited clusters with Df =1.4 and then lines up to Von Koch curve with random interval with Df=1.14. Here, our goal is to try to interpret the low conductivity and/or broad forbidden gap of GO doped PAAm gels, by the distribution of GO in the final form of the produced gel.

Keywords: composite gels, fluorescence, fractal, scaling

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Authors: Selim Kara, Ertan Arda, Fahrettin Dolastir, Önder Pekcan

Abstract:

Biomaterials and thin film coatings play a fundamental role in medical, food and pharmaceutical industries. Carrageenan is a linear sulfated polysaccharide extracted from algae and seaweeds. To date, such biomaterials have been used in many smart drug delivery systems due to their biocompatibility and antimicrobial activity properties. Poly (N-isopropylacrylamide) (PNIPAm) gels and copolymers have also been used in medical applications. PNIPAm shows lower critical solution temperature (LCST) property at about 32-34 °C which is very close to the human body temperature. Below and above the LCST point, PNIPAm gels exhibit distinct phase transitions between swollen and collapsed states. A special class of gels are microgels which can react to environmental changes significantly faster than microgels due to their small sizes. Quartz crystal microbalance (QCM) measurement technique is one of the attractive techniques which has been used for monitoring the thin-film formation process. A sensitive QCM system was designed as to detect 0.1 Hz difference in resonance frequency and 10-7 change in energy dissipation values, which are the measures of the deposited mass and the film rigidity, respectively. PNIPAm microgels with the diameter around few hundred nanometers in water were produced via precipitation polymerization process. 5 MHz quartz crystals with functionalized gold surfaces were used for the deposition of the carrageenan molecules and microgels in the solutions which were slowly pumped through a flow cell. Interactions between charged carrageenan and microgel particles were monitored during the formation of the film layers, and the Sauerbrey masses of the deposited films were calculated. The critical phase transition temperatures around the LCST were detected during the heating and cooling cycles. It was shown that it is possible to monitor the interactions between PNIPAm microgels and biopolymer molecules, and it is also possible to specify the critical phase transition temperatures by using a QCM system.

Keywords: carrageenan, phase transitions, PNIPAm microgels, quartz crystal microbalance (QCM)

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Authors: Yogita Patil-Sen

Abstract:

Superparamagnetic Iron Oxide Nanoparticles (SPIONs) have become increasingly important materials for separation of specific bio-molecules, drug delivery vehicle, contrast agent for MRI and magnetic hyperthermia for cancer therapy. Hyperthermia is emerging as an alternative cancer treatment to the conventional radio- and chemo-therapy, which have harmful side effects. When subjected to an alternating magnetic field, the magnetic energy of SPIONs is converted into thermal energy due to movement of particles. The ability of SPIONs to generate heat and potentially kill cancerous cells, which are more susceptible than the normal cells to temperatures higher than 41 °C forms the basis of hyerpthermia treatement. The amount of heat generated depends upon the magnetic properties of SPIONs which in turn is affected by their properties such as size and shape. One of the main problems associated with SPIONs is particle aggregation which limits their employability in in vivo drug delivery applications and hyperthermia cancer treatments. Coating the iron oxide core with thermally responsive lipid based nanostructures tend to overcome the issue of aggregation as well as improve biocompatibility and can enhance drug loading efficiency. Herein we report suitability of SPIONs and silica coated core-shell SPIONs, which are further, coated with various lipids for drug delivery and magnetic hyperthermia applications. The synthesis of nanoparticles is carried out using the established methods reported in the literature with some modifications. The nanoparticles are characterised using Infrared spectroscopy (IR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Vibrating Sample Magnetometer (VSM). The heating ability of nanoparticles is tested under alternating magnetic field. The efficacy of the nanoparticles as drug carrier is also investigated. The loading of an anticancer drug, Doxorubicin at 18 °C is measured up to 48 hours using UV-visible spectrophotometer. The drug release profile is obtained under thermal incubation condition at 37 °C and compared with that under the influence of alternating magnetic field. The results suggest that the nanoparticles exhibit superparamagnetic behaviour, although coating reduces the magnetic properties of the particles. Both the uncoated and coated particles show good heating ability, again it is observed that coating decreases the heating behaviour of the particles. However, coated particles show higher drug loading efficiency than the uncoated particles and the drug release is much more controlled under the alternating magnetic field. Thus, the results demonstrate that lipid coated SPIONs exhibit potential as drug delivery vehicles for magnetic hyperthermia based cancer therapy.

Keywords: drug delivery, hyperthermia, lipids, superparamagnetic iron oxide nanoparticles (SPIONS)

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Authors: Yogita Patil-Sen

Abstract:

Magnetic nanoparticles such as those made of iron oxide have been widely explored as biocatalysts, contrast agents, and drug delivery systems. However, some of the challenges associated with these particles are agglomeration and biocompatibility, which lead to concern of toxicity of the particles, especially for drug delivery applications. Coating the particles with biocompatible materials such as lipids and peptides have shown to improve the mentioned issues. Thus, these core-shell type nanoparticles are emerging as the new class of nanomaterials for targeted drug delivery applications. In this study, various types of core-shell magnetic nanoparticles are prepared and characterized using techniques, such as Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Vibrating Sample Magnetometer (VSM) and Thermogravimetric Analysis (TGA). The heating ability of nanoparticles is tested under oscillating magnetic field. The efficacy of the nanoparticles as drug carrier is also investigated. The loading of an anticancer drug, Doxorubicin at 18 °C is measured up to 48 hours using UV-visible spectrophotometer. The drug release profile is obtained under thermal incubation condition at 37 °C and compared with that under the influence of oscillating field. The results suggest that the core-shell nanoparticles exhibit superparamagnetic behaviour, although, coating reduces the magnetic properties of the particles. Both the uncoated and coated particles show good heating ability, again it is observed that coating decreases the heating behaviour of the particles. However, coated particles show higher drug loading efficiency than the uncoated particles and the drug release is much more controlled under the oscillating magnetic field. Thus, the results strongly indicate the suitability of the prepared core-shell type nanoparticles as drug delivery vehicles and their potential in magnetic hyperthermia applications and for hyperthermia cancer therapy.

Keywords: core-shell, hyperthermia, magnetic nanoparticles, targeted drug delivery

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Authors: S. Al-Enezi, J. Samuel, A. Al-Banna

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Polymer based membranes are one of the low-cost technologies available for the gas separation. Three major elements required for a commercial gas separating membrane are high permeability, high selectivity, and good mechanical strength. Poly(vinylidene fluoride) (PVDF) is a commercially available fluoropolymer and a widely used membrane material in gas separation devices since it possesses remarkable thermal, chemical stability, and excellent mechanical strength. The PVDF membrane was chemically modified by soaking in different ionic liquids and dried. The thermal behavior of modified membranes was investigated by differential scanning calorimetry (DSC), and thermogravimetry (TGA), and the results clearly show the best affinity between the ionic liquid and the polymer support. The porous structure of the PVDF membranes was clearly seen in the scanning electron microscopy (SEM) images. The CO₂ permeability of blended membranes was explored in comparison with the unmodified matrix. The ionic liquid immobilized in the hydrophobic PVDF support exhibited good performance for separations of CO₂/N₂. The improved permeability of modified membrane (PVDF-IL) is attributed to the high concentration of nitrogen rich imidazolium moieties.

Keywords: PVDF, polymer membrane, gas permeability, CO₂ separation, nanotubes

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Authors: Mihai-Alexandru Florea, Veronica Drumea, Roxana Nita, Cerasela Gird, Laura Olariu

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The aim of this study was to investigate the residues of pesticide found in tea water infusions. A multi-residues method to determine 147 pesticides has been developed using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) procedure and dispersive solid phase extraction (d-SPE) for the cleanup the pesticides from complex matrices such as plants and tea. Sample preparation was carefully optimized for the efficient removal of coextracted matrix components by testing more solvent systems. Determination of pesticides was performed using GC-MS/MS (100 of pesticides) and LC-MS/MS (47 of pesticides). The selected reaction monitoring (SRM) mode was chosen to achieve low detection limits and high compounds selectivity and sensitivity. Overall performance was evaluated and validated according to DG-SANTE Guidelines. To assess the pesticide residue transfer rate (qualitative) from dried tea in infusions the samples (tea) were spiked with a mixture of pesticides at the maximum residues level accepted for teas and herbal infusions. In order to investigate the release of the pesticides in tea preparations, the medicinal plants were prepared in four ways by variation of water temperature and the infusion time. The pesticides from infusions were extracted using two methods: QuEChERS versus solid-phase extraction (SPE). More that 90 % of the pesticides studied was identified in infusion.

Keywords: tea, solid-phase extraction (SPE), selected reaction monitoring (SRM), QuEChERS

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Authors: Francisco Espinosa, Juan Chavarría

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Glycerol is a byproduct of biodiesel production that can be used for aqueous-phase reforming to obtain hydrogen. Iridium is a material that has high activity and hydrogen selectivity for steam phase reforming. Nevertheless, a drawback for the use of iridium in aqueous-phase reforming is the low activity in water-gas shift reaction. Therefore, in this work, it is proposed the use of nickel and copper as a second metal in the catalyst to reach a synergetic effect. Iridium, iridium-nickel and iridium-copper catalysts were prepared by incipient wetness impregnation and evaluated in the aqueous-phase reforming of glycerol using CeO₂ or La₂O₃ as support. The catalysts were characterized by XRD, XPS, and EDX. The reactions were carried out in a fixed bed reactor feeding a solution of glycerol 10 wt% in water at 270°C, and reaction products were analyzed by gas chromatography. It was found that IrNi/CeO₂ reached highest glycerol conversion and hydrogen production, slightly above 70% and 43 vol% respectively. In terms of conversion, iridium is a promising metal, and its activity for hydrogen production can be enhanced when adding a second metal.

Keywords: aqueous-phase reforming, glycerol, hydrogen production, iridium

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Authors: Iftikhar Ahmad, Mohammad Islam

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Thermally exfoliated graphene nanomaterial was reinforced into Al2O3 ceramic and the nanocomposites were consolidated using rapid high-frequency induction heat sintering route. The resulting nanocomposites demonstrated higher mechanical properties due to efficient GNS incorporation and chemical interaction with the Al2O3 matrix grains. The enhancement in mechanical properties is attributed to (i) uniformly-dispersed GNS in the consolidated structure (ii) ability of GNS to decorate Al2O3 nanoparticles and (iii) strong GNS/Al2O3 chemical interaction during colloidal mixing and pullout/crack bridging toughening mechanisms during mechanical testing. The GNS/Al2O3 interaction during different processing stages was thoroughly examined by thermal and structural investigation of the interfacial area. The formation of an intermediate aluminum oxycarbide phase (Al2OC) via a confined carbothermal reduction reaction at the GNS/Al2O3 interface was observed using advanced electron microscopes. The GNS surface roughness improves GNS/Al2O3 mechanical locking and chemical compatibility. The sturdy interface phase facilitates efficient load transfer and delayed failure through impediment of crack propagation. The resulting nanocomposites, therefore, offer superior toughness.

Keywords: ceramics, nanocomposites, interfaces, nanostructures, electron microscopy, Al2O3

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Authors: Lisa Shambare, Jean Mulopo, Sehliselo Ndlovu

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One of the major challenges of sustainable development is promoting an industry which is both ecologically durable and economically viable. This requires processes that are material and energy efficient whilst also being able to limit the production of waste and toxic effluents through effective methods of process synthesis and intensification. In South Africa and globally, both miniaturisation and technological advances have substantially increased the amount of electronic wastes (e-waste) generated annually. Vast amounts of e-waste are being generated yearly with only a minute quantity being recycled officially. The passion for electronic devices cannot ignore the scarcity and cost of mining the noble metal resources which contribute significantly to the efficiency of most electronic devices. It has hence become imperative especially in an African context that sustainable strategies which are environmentally friendly be developed for recycling of the noble metals from e-waste. This paper investigates the recovery of gold, silver and palladium from electronic wastes, which consists of a vast array of metals, using ionic liquids which have the potential of reducing the gaseous and aqueous emissions associated with existing hydrometallurgical and pyrometallurgical technologies while also maintaining the economy of the overall recycling scheme through solvent recovery. The ionic liquids 1-butyl-3-methyl imidazolium hydrogen sulphate (BmimHSO4) which behaves like a protic acid and was used in the present research for the selective leaching of gold and silver from e-waste. Different concentrations of the aqueous ionic liquid were used in the experiments ranging from 10% to 50%. Thiourea was used as the complexing agent in the investigation with Fe3+ as the oxidant. The pH of the reaction was maintained in the range of 0.8 to 1.5. The preliminary investigations conducted were successful in the leaching of silver and palladium at room temperature with optimum results being at 48hrs. The leaching results could not be explained because of the leaching of palladium with the absence of gold. Hence a conclusion could not be drawn and there was the need for further experiments to be run. The leaching of palladium was carried out with hydrogen peroxide as oxidant and 1-butyl-3-methyl imidazolium chloride (BmimCl) as the solvent. The experiments at carried out at a temperature of 60 degrees celsius and a very low pH. The chloride ion was used to complex with palladium metal. From the preliminary results, it could be concluded that pretreatment of the treatment e-waste was necessary to improve the efficiency of the metal recovery process. A conclusion could not be drawn for the leaching experiments.

Keywords: BmimCl, BmimHSO4, gold, palladium, silver

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Authors: S. Fröhlich, M. Herold, M. Allmer

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Early stage quantitative analysis of host cell protein (HCP) variations is challenging yet necessary for comprehensive bioprocess development. High resolution mass spectrometry (HRMS) provides a high-end technology for accurate identification alongside with quantitative information. Hereby we describe a flexible HRMS assay platform to quantify HCPs relevant in microbial expression systems such as E. Coli in both up and downstream development by means of MVDA tools. Cell pellets were lysed and proteins extracted, purified samples not further treated before applying the SMART tryptic digest kit. Peptides separation was optimized using an RP-UHPLC separation platform. HRMS-MSMS analysis was conducted on an Orbitrap Velos Elite applying CID. Quantification was performed label-free taking into account ionization properties and physicochemical peptide similarities. Results were analyzed using SIEVE 2.0 (Thermo Fisher Scientific) and SIMCA (Umetrics AG). The developed HRMS platform was applied to an E. Coli expression set with varying productivity and the corresponding downstream process. Selected HCPs were successfully quantified within the fmol range. Analysing HCP networks based on pattern analysis facilitated low level quantification and enhanced validity. This approach is of high relevance for high-throughput screening experiments during upstream development, e.g. for titer determination, dynamic HCP network analysis or product characterization. Considering the downstream purification process, physicochemical clustering of identified HCPs is of relevance to adjust buffer conditions accordingly. However, the technology provides an innovative approach for label-free MS based quantification relying on statistical pattern analysis and comparison. Absolute quantification based on physicochemical properties and peptide similarity score provides a technological approach without the need of sophisticated sample preparation strategies and is therefore proven to be straightforward, sensitive and highly reproducible in terms of product characterization.

Keywords: process analytical technology, mass spectrometry, process characterization, MVDA, pattern recognition

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Authors: Ramalingam Boobalan, Chinpiao Chen, Jui-I. Chiao

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A series of erlotinib analogues that have structural modification at 6,7-alkoxyl positions is efficiently synthesized. The key reactions that involved in synthesis are one-pot oxime formation-dehydration for the formation of nitrile, quinazoline ring formation reaction between aniline and o-cyanoaniline via formamidine intermediate, Fe/NH4Cl catalyzed reduction-hetereocyclization-reductive ring opening reaction for the formation of o-aminobenzamide, high yielding seal tube reactions for O-demethylation, sodium iodide substitution, ammonia substitution. The in vitro anti-tumor activity of synthesized compounds is studied in two non-small cell lung cancer (NSCLC) cell lines (A549 and H1975). Among the synthesized compounds, the iodo compound 6 (ETN-6) exhibits higher anti-cancer activity compared to erlotinib. An efficient method is developed for the conjugation of erlotinib analogue-4, alcohol compound, with protein, bovine serum albumin (BSA), via succinic acid linker. The in vitro anti-tumor activity of the protein attached erlotinib analogue, 8 (ETN-4-Suc-BSA), showed stronger inhibitory activity in both A549 and H1975 NSCLC cell lines.

Keywords: anti-cancer, BSA, EGFR, Erlotinib

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Authors: Istvan Szilagyi, Marko Pavlovic, Paul Rouster

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Antioxidant enzymes are the most efficient defense systems against reactive oxygen species, which cause severe damage in living organisms and industrial products. However, their supplementation is problematic due to their high sensitivity to the environmental conditions. Immobilization on carrier nanoparticles is a promising research direction towards the improvement of their functional and colloidal stability. In that way, their applications in biomedical treatments and manufacturing processes in the food, textile and cosmetic industry can be extended. The main goal of the present research was to prepare and formulate antioxidant bionanocomposites composed of superoxide dismutase (SOD) enzyme, anionic clay (layered double hydroxide, LDH) nanoparticle and heparin (HEP) polyelectrolyte. To characterize the structure and the colloidal stability of the obtained compounds in suspension and solid state, electrophoresis, dynamic light scattering, transmission electron microscopy, spectrophotometry, thermogravimetry, X-ray diffraction, infrared and fluorescence spectroscopy were used as experimental techniques. LDH-SOD composite was synthesized by enzyme immobilization on the clay particles via electrostatic and hydrophobic interactions, which resulted in a strong adsorption of the SOD on the LDH surface, i.e., no enzyme leakage was observed once the material was suspended in aqueous solutions. However, the LDH-SOD showed only limited resistance against salt-induced aggregation and large irregularly shaped clusters formed during short term interval even at lower ionic strengths. Since sufficiently high colloidal stability is a key requirement in most of the applications mentioned above, the nanocomposite was coated with HEP polyelectrolyte to develop highly stable suspensions of primary LDH-SOD-HEP particles. HEP is a natural anticoagulant with one of the highest negative line charge density among the known macromolecules. The experimental results indicated that it strongly adsorbed on the oppositely charged LDH-SOD surface leading to charge inversion and to the formation of negatively charged LDH-SOD-HEP. The obtained hybrid materials formed stable suspension even under extreme conditions, where classical colloid chemistry theories predict rapid aggregation of the particles and unstable suspensions. Such a stabilization effect originated from electrostatic repulsion between the particles of the same sign of charge as well as from steric repulsion due to the osmotic pressure raised during the overlap of the polyelectrolyte chains adsorbed on the surface. In addition, the SOD enzyme kept its structural and functional integrity during the immobilization and coating processes and hence, the LDH-SOD-HEP bionanocomposite possessed excellent activity in decomposition of superoxide radical anions, as revealed in biochemical test reactions. In conclusion, due to the improved colloidal stability and the good efficiency in scavenging superoxide radical ions, the developed enzymatic system is a promising antioxidant candidate for biomedical or other manufacturing processes, wherever the aim is to decompose reactive oxygen species in suspensions.

Keywords: clay, enzyme, polyelectrolyte, formulation

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Authors: Hellal Abdelkader, Chafaa Salah, Touafri Lasnouni

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A simple, efficient and general method has been developed for the high diastereoselective synthesis of diethyl α-aminophosphonates in water through “one-pot” three-component reaction of aromatic aldehydes, aminophenols and dialkyl phosphites in the presence of a low catalytic amount (10mol%) of phosphorous acid as highly stable catalyst is described.

Keywords: DFT, HOMO-LUMO, phosphonic acid, aminophenols

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Authors: Yu-Wei Chang, Hsuan-Yu Ku, Jo-Shan Chiu, Shao-Fu Chang, Chien-Chon Chen

Abstract:

This paper aims to discuss the hydrophilicity about the anodic aluminum oxide (AAO) template with titania nanotubes (NTs). The AAO templates with pore size diameters of 20-250 nm were generated by anodizing 6061 aluminum alloy substrates in acid solution of sulfuric acid (H₂SO₄), oxalic acid (COOH)₂, and phosphoric acid (H₃PO₄), respectively. TiO₂-NTs were grown on AAO templates by the sol-gel deposition process successfully. The water contact angle on AAO/TiO₂-NTs surface was lower compared to the water contact angle on AAO surface. So, the characteristic of hydrophilicity was significantly associated with the AAO pore size and what kinds of materials were immersed variables.

Keywords: AAO, nanotube, sol-gel, anodization, hydrophilicity

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Authors: Chanho Park, Juneseok You, Kuewhan Jang, Sungsoo Na

Abstract:

Detection technique of nanotoxic materials is strongly imperative, because nano-toxic materials can harmfully influence human health and environment as their engineering applications are growing rapidly in recent years. In present work, we report the DNA immobilized quartz crystal microbalance (QCM) based sensor for detection of nano-toxic materials such as silver ions, Hg2+ etc. by using functionalization of quartz crystal with a target-specific DNA. Since the mass of a target material is comparable to that of an atom, the mass change caused by target binding to DNA on the quartz crystal is so small that it is practically difficult to detect the ions at low concentrations. In our study, we have demonstrated fast and in situ detection of nanotoxic materials using quartz crystal microbalance. We report the label-free and highly sensitive detection of silver ion for present case, which is a typical nano-toxic material by using QCM and silver-specific DNA. The detection is based on the measurement of frequency shift of Quartz crystal from constitution of the cytosine-Ag+-cytosine binding. It is shown that the silver-specific DNA measured frequency shift by QCM enables the capturing of silver ions below 100pM. The results suggest that DNA-based detection opens a new avenue for the development of a practical water-testing sensor.

Keywords: nano-toxic ions, quartz crystal microbalance, frequency shift, target-specific DNA

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Authors: Vigen Barkhudaryan

Abstract:

The influence of external effects (γ-, UV–radiations, high temperature) in presence of air oxygen on structural transformations of low-density polyethylene (LDPE) have been investigated dependent on the polymers’ thickness, the intensity and the dose of external actions. The methods of viscosimetry, light scattering, turbidimetry and gelation measuring were used for this purpose. The comparison of influence of external effects on LDPE shows, that the destruction and cross-linking processes of macromolecules proceed simultaneously with all kinds of external effects. A remarkable growth of average molecular mass of LDPE along with the irradiation doses and heat treatment exposure growth was established. It was linear for the mass average molecular mass and at the initial doses is mainly the result of the increase of the macromolecular branching. As a result, the macromolecular hydrodynamic volumes have been changed, and therefore the dependence of viscosity average molecular mass on the doses was going through the minimum at initial doses. A significant change of molecular mass, sizes and shape of macromolecules of LDPE occurs under the influence of external effects. The influence is limited only by diffusion of oxygen during -irradiation and heat treatment. At UV–irradiation the influence is limited both by diffusion of oxygen and penetration of radiation. Consequently, the molecular transformations are deeper and evident in case of -irradiation, as soon as the polymer is transformed in a whole volume. It was also established, that the mechanism of molecular transformations in polymers from the surface layer distinctly differs from those of the sample deeper layer. A comparison of the results of these investigations allows us to conclude, that the mechanisms of influence of investigated external effects on polyethylene are similar.

Keywords: cross-linking, destruction, high temperature, LDPE, γ-radiations, UV-radiations

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Authors: Chien-Wan Hun, Shao-Fu Chang, Chien-Chon Chen, Ker-Jer Huang

Abstract:

This study presents how to use a high-efficiency process for producing cesium iodide (CsI) crystal columns by rapid heating method. In the past, the heating rate of the resistance wire heating furnace was relatively slow and excessive iodine and CsI vapors were therefore generated during heating. Because much iodine and CsI vapors are produced during heating process, the composition of CsI crystal columns is not correct. In order to enhance the heating rate, making CsI material in the heating process can quickly reach the melting point temperature. This study replaced the traditional type of external resistance heating furnace with halogen-type quartz heater, and then, CsI material can quickly reach the melting point. Eventually, CsI melt can solidify in the anodic aluminum template forming CsI crystal columns.

Keywords: cesium iodide, high efficiency, vapor, rapid heating, crystal column

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Authors: I. Grigoraviciute-Puroniene, K. Tsuru, E. Garskaite, Z. Stankeviciute, A. Beganskiene, K. Ishikawa, A. Kareiva

Abstract:

Tricalcium phosphate (β-Ca₃(PO₄)₂, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.

Keywords: Tricalcium phosphate (β-Ca3(PO4)2, bone regeneration, wet chemical processing, polymeric precipitation

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Authors: Dilip Saikia, Suparna Bhattacharjee, Nirab Adhikary

Abstract:

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

Keywords: photoluminescence, quantum dots, quenching, sensor

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Authors: H. K. Shahzad, M. A. Hussein, F. Patel, N. Al-Aqeeli, T. Laoui

Abstract:

The purpose of the present study was to use the adsorption mechanism with microfiltration synergistically for efficient heavy metal removal from contaminated water. Alumina (Al2O3) is commonly used for ceramic membranes development while recently carbon nanotubes (CNTs) have been considered among the best adsorbent materials for heavy metals. In this work, we combined both of these materials to prepare porous Al2O3-CNTs nanocomposite membranes via Spark Plasma Sintering (SPS) technique. Alumina was used as a base matrix while CNTs were added as filler. The SPS process parameters i.e. applied pressure, temperature, heating rate, and holding time were varied to obtain the best combination of porosity (64%, measured according to ASTM c373-14a) and strength (3.2 MPa, measured by diametrical compression test) of the developed membranes. The prepared membranes were characterized using X-ray diffraction (XRD), field emission secondary electron microscopy (FE-SEM), contact angle and porosity measurements. The results showed that properties of the synthesized membranes were highly influenced by the SPS process parameters. FE-SEM images revealed that CNTs were reasonably dispersed in the alumina matrix. The porous membranes were evaluated for their water flux transport as well as their capacity to adsorb heavy metals ions. Selected membranes were able to remove about 97% cadmium from contaminated water. Further work is underway to enhance the removal efficiency of the developed membranes as well as to remove other heavy metals such as arsenic and mercury.

Keywords: heavy metal removal, inorganic membrane, nanocomposite, spark plasma sintering

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Authors: Dana A. Thal, Heike Kahlert, Fritz Scholz

Abstract:

Thiol molecules are known to easily form self-assembled monolayers (SAM) on Au surfaces. Depending on the thiol’s structure, surface modifications via SAM can be used for electrode sensor development. In the presented work, 1-decanethiol coated polycrystalline Au electrodes were applied to indirectly assess the radical scavenging potential of plant compounds and extracts. Different plant compounds with reported antioxidant properties as well as an extract from the plant Gynostemma pentaphyllum were tested for their effectiveness to prevent SAM degradation on the sensor electrodes via photolytically generated radicals in aqueous media. The SAM degradation was monitored over time by differential pulse voltammetry (DPV) measurements. The results were compared to established antioxidant assays. The obtained data showed an exposure time and concentration dependent degradation process of the SAM at the electrode’s surfaces. The tested substances differed in their capacity to prevent SAM degradation. Calculated radical scavenging activities of the tested plant compounds were different for different assays. The presented method poses a simple system for radical scavenging evaluation and, considering the importance of the test system in antioxidant activity evaluation, might be taken as a bridging tool between in-vivo and in-vitro antioxidant assay in order to obtain more biologically relevant results in antioxidant research.

Keywords: alkanethiol SAM, plant antioxidant, polycrystalline Au, radical scavenger

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Authors: Francesca Risplendi, Li-Chiang Lin, Jeffrey C. Grossman, Giancarlo Cicero

Abstract:

Desalination is one of the most employed approaches to supply water in the context of a rapidly growing global water shortage. However, the most popular water filtration method available is the reverse osmosis (RO) technique, still suffers from important drawbacks, such as a large energy demands and high process costs. In addition some serious limitations have been recently discovered, among them, the boron problem seems to have a critical meaning. Boron has been found to have a dual effect on the living systems on Earth and the difference between boron deficiency and boron toxicity levels is quite small. The aim of this project is to develop a new generation of RO membranes based on porous graphene or reduced graphene oxide (rGO) able to remove salts from seawater and to reduce boron concentrations in the permeate to the level that meets the drinking or process water requirements, by means of a theoretical approach based on density functional theory and classical molecular dynamics. Computer simulations have been employed to investigate the relationship between the atomic structure of nanoporous graphene or rGO monolayer and its membrane properties in RO applications (i.e. water permeability and resilience at RO pressures). In addition, an emphasis has been given to multilayer nanoporous rGO and rGO flakes based membranes. By means of non-equilibrium MD simulations, we investigated the water transport mechanism permeating through such multilayer membrane focusing on the effect of slit widths and sheet geometries. These simulations allowed us to establish the implications of these graphene based materials as promising membrane properties for desalination plants and as boron filtration.

Keywords: boron filtration, desalination, graphene membrane, reduced graphene oxide membrane

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Authors: Bartosz Piechowicz, Stanislaw Sadlo, Przemyslaw Grodzicki, Magdalena Podbielska

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Apples are popular fruits. They are eaten freshly and/or after processing. For instance Golden Delicious is an apple variety commonly used in production of foods for babies and toddlers. It is no wonder that complex analyses of the pesticide residue levels in those fruits have been carried out since eighties, and continued for the next years up to now. The results obtained were presented, usually as a teamwork, at the scientific sessions organised by the (IOR) Institute of Plant Protection-National Research Institute in Poznań and published in Scientific Works of the Institute (now Progress in Plant Protection/ Postępy w Ochronie Roślin) or Journal of Plant Protection Research, and in many non-periodical publications. These reports included studies carried out by IOR Laboratories in Poznań, Sośnicowice, Rzeszów and Bialystok. First detailed studies on the presence of pesticide residues in apple fruits by the laboratory in Rzeszów were published in 1991 in the article entitled 'The presence of pesticides in apples of late varieties from the area of south-eastern Poland in the years 1986-1989', in Annals of National Institute of Hygiene in Warsaw. These surveys gave the scientific base for business contacts between the Polish company Alima and the American company Gerber. At the beginning of XXI century, in Poland, systematic and complex studies on the deposition of pesticide residues in apples were initiated. First of all, the levels of active ingredients of plant protection products applied against storage diseases at 2-3 weeks before the harvest were determined. It is known that the above mentioned substances usually generate the highest residue levels. Also, the assessment of the fungicide residues in apples during their storage in controlled atmosphere and during their processing was carried out. Taking into account the need of actualisation the Maximum Residue Levels of pesticides, in force in Poland and in other European countries, and rationalisation of the ways of their determination, a lot of field tests on the behaviour of more important fungicides on the mature fruits just before their harvesting, were carried out. A rate of their disappearance and mathematical equation that showed the relationship between the residue level of any substance and the used dose, have been determined. The two parameters have allowed to evaluate the Maximum Residue Levels (MRLs) of pesticides, which were in force at that time, and to propose a coherent model of their determination in respect to the new substances. The obtained results were assessed in terms of the health risk for adult consumers and children, and to such determination of terms of treatment that mature apples could meet the rigorous level of 0.01 mg/kg.

Keywords: apple, disappearance, health risk, MRL, pesticide residue, research

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Authors: Zeynep Dikmen, Vural Bütün

Abstract:

Electron donor or acceptor capability to participate in electron conjugation is the requirement for an electroactive material. Conjugated molecules and polymers bearing heterocyclic units have potential as optically electroactive materials. Thiazolo thiazole based compounds have attention for last two decades, because they have attractive electronic and optical properties, these compounds are useful for electronic application areas such as dye sentisized solar cells (DSSCs), organic light emitting diodes (OLEDs) and field effect transistors (FETs). Thiazolo[5,4-d]thiazole is bicyclic aromatic structure contains N and S atoms which act as electron donor. A new electron accepting or donating group bound to thiazolo [5,4-d] thiazole fused ring can change the electronic, spectroscopic, stability and dyeing properties of the new material. Polyphenylene(thiazolo [5,4-d] thiazole) (p-PhTT) compound was synthesized via condensation reaction of terephthalaldehyde with dithiooxamide. The chemical structure was determined with solid state 13C NMR spectroscopy. Optical properties (i.e. absorbance and band gap) was determined via solid UV-vis spectroscopy. The insoluble polymer was quarternized with 4-vinylbenzyl chloride (VBC). Colorless VBC changed into a yellow liquid. AgNO3 complex were prepared and optical properties were investigated with UV-Vis, fluorescence spectroscopy and X-ray spectroscopy and cyclic voltammetry studies were examined in this research. This structure exhibits good absorbance and fluorescence in UV-vis region. Synthesis scheme of PyTT and preparation of metal complexes are given. PyTT has absorbance at ~360 nm and fluorescence at ~420 nm.

Keywords: thiazolo thiazole, quarternized polymers, polymeric ligands, Ag complexes

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Authors: Shashikant R. Kuchekar, Shivaji D. Pulate, Vishwas B. Gaikwad

Abstract:

A simple and selective method is developed for solvent extraction spectrophotometric determination of antimony(III) using O-Methylphenyl Thiourea (OMPT) as a sensitive chromogenic chelating agent. The basis of proposed method is formation of antimony(III)-OMPT complex was extracted with 0.0025 M OMPT in chloroform from aqueous solution of antimony(III) in 1.0 M perchloric acid. The absorbance of this complex was measured at 297 nm against reagent blank. Beer’s law was obeyed up to 15µg mL-1 of antimony(III). The Molar absorptivity and Sandell’s sensitivity of the antimony(III)-OMPT complex in chloroform are 16.6730 × 103 L mol-1 cm-1 and 0.00730282 µg cm-2 respectively. The stoichiometry of antimony(III)-OMPT complex was established from slope ratio method, mole ratio method and Job’s continuous variation method was 1:2. The complex was stable for more than 48 h. The interfering effect of various foreign ions was studied and suitable masking agents are used wherever necessary to enhance selectivity of the method. The proposed method is successfully applied for determination of antimony(III) from real samples alloy and synthetic mixtures. Repetition of the method was checked by finding relative standard deviation (RSD) for 10 determinations which was 0.42%.

Keywords: solvent extraction, antimony, spectrophotometry, real sample analysis

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Authors: Rodrigo Antunes, Olga Borisevich, David Demange

Abstract:

In future nuclear fusion reactors, tritium self-sufficiency will be ensured by tritium (3H) production via reactions between the fusion neutrons and lithium. To favor tritium breeding, a neutron multiplier must also be used. Both tritium breeder and neutron multiplier will be placed in the so-called Breeding Blanket (BB). For the European Helium-Cooled Pebble Bed (HCPB) BB concept, the tritium production and neutron multiplication will be ensured by neutron bombardment of Li4SiO4 and Be pebbles, respectively. The produced tritium is extracted from the pebbles by purging them with large flows of He (~ 104 Nm3h-1), doped with small amounts of H2 (~ 0.1 vol%) to promote tritium extraction via isotopic exchange (producing HT). Due to the presence of oxygen in the pebbles, production of tritiated water is unavoidable. Therefore, the purging gas downstream of the BB will be composed by Q2/Q2O/He (Q = 1H, 2H, 3H), with Q2/Q2O down to ppm levels, which must be further processed for tritium recovery. A two-stage continuous approach, where zeolite membranes (ZMs) are followed by a catalytic membrane reactor (CMR), has been recently proposed to fulfil this task. The tritium recovery from Q2/Q2O/He is ensured by the CMR, that requires a reduction of the gas flow coming from the BB and a pre-concentration of Q2 and Q2O to be efficient. For this reason, and to keep this stage with reasonable dimensions, ZMs are required upfront to reduce as much as possible the He flows and concentrate the Q2/Q2O species. Therefore, experimental activities have been carried out at the Tritium Laboratory Karlsruhe (TLK) to test the separation performances of different zeolite membranes for H2/H2O/He. First experiments have been performed with binary mixtures of H2/He and H2O/He with commercial MFI-ZSM5 and NaA zeolite-type membranes. Only the MFI-ZSM5 demonstrated selectivity towards H2, with a separation factor around 1.5, and H2 permeances around 0.72 µmolm-2s-1Pa-1, rather independent for feed concentrations in the range 0.1 vol%-10 vol% H2/He. The experiments with H2O/He have demonstrated that the separation factor towards H2O is highly dependent on the feed concentration and temperature. For instance, at 0.2 vol% H2O/He the separation factor with NaA is below 2 and around 1000 at 5 vol% H2O/He, at 30°C. Overall, both membranes demonstrated complementary results at equivalent temperatures. In fact, at low feed concentrations ( ≤ 1 vol% H2O/He) MFI-ZSM5 separates better than NaA, whereas the latter has higher separation factors for higher inlet water content ( ≥ 5 vol% H2O/He). In this contribution, the results obtained with both MFI-ZSM5 and NaA membranes for H2/He and H2O/H2 mixtures at different concentrations and temperatures are compared and discussed.

Keywords: nuclear fusion, gas separation, tritium processes, zeolite membranes

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Authors: Rouzbeh Ramezani, Renzo Di Felice

Abstract:

Nowadays, removal of CO₂ as one of the major contributors to global warming using alternative solvents with high CO₂ absorption efficiency, is an important industrial operation. In this study, three amines, including 2-methylpiperazine, potassium sarcosinate and potassium lysinate as potential additives, were added to the potassium carbonate solution as a base solvent for CO₂ capture. In order to study the absorption performance of CO₂ in terms of loading capacity of CO₂ and absorption rate, the absorption experiments in a blend of additives with potassium carbonate were carried out using the vapor-liquid equilibrium apparatus at a temperature of 313.15 K, CO₂ partial pressures ranging from 0 to 50 kPa and at mole fractions 0.2, 0.3, and 0.4. Furthermore, the performance of CO₂ absorption in these blend solutions was compared with pure monoethanolamine and with pure potassium carbonate. Finally, a correlation with good accuracy was developed using the nonlinear regression analysis in order to predict CO₂ loading capacity.

Keywords: absorption rate, carbon dioxide, CO2 capture, global warming, loading capacity

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Authors: Daihui Zhang, Marie J. Dumont

Abstract:

A derivative of 5-hydroxymethylfurfural (HMF) was synthesized for the thiol-Michael addition reaction. The efficiency of the catalysts (base and nucleophiles) and side reactions during the thiol-Michael addition were investigated. Dimethylphenylphosphine efficiently initiated the thiol-Michael addition polymerization for synthesizing a series of bio-based furan polymers with different structure and properties. The benzene rings or hydroxyl groups present in the polymer chains increased the glass transition temperature (Tg) of poly (β-thioether ester). Additionally, copolymers with various compositions were obtained via adding different ratio of 1,6-hexanedithiols to 1,4-benzenedithiols. 1H NMR analysis revealed that experimental ratios of two dithiols monomers matched well with theoretical ratios. The occurrence of a reversible Diels-Alder reaction between furan rings and maleimide groups allowed poly (β-thioether ester) to be dynamically crosslinked. These polymers offer the potentials to produce materials from biomass that have both practical mechanical properties and reprocessing ability.

Keywords: copolymers, Diels-Alder reaction, hydroxymethylfurfural, Thiol-Michael addition

Procedia PDF Downloads 331