Search results for: spectroscopy

Authors: Uttam Kumar Ghorai, Madhupriya Samanta, Subhajit Saha, Swati Das, Nilesh Mazumder, Kalyan Kumar Chattopadhyay

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Organic semiconductors have gained potential interest in the last few decades for their significant contributions in the various fields such as solar cell, non-volatile memory devices, field effect transistors and light emitting diodes etc. The most important advantages of using organic materials are mechanically flexible, light weight and low temperature depositing techniques. Recently with the advancement of nanoscience and technology, one dimensional organic and inorganic nanostructures such as nanowires, nanorods, nanotubes have gained tremendous interests due to their very high aspect ratio and large surface area for electron transport etc. Among them, self-assembled organic nanostructures like Copper, Zinc Phthalocyanine have shown good transport property and thermal stability due to their π conjugated bonds and π-π stacking respectively. Field emission properties of inorganic and carbon based nanostructures are reported in literatures mostly. But there are few reports in case of cold cathode emission characteristics of organic semiconductor nanostructures. In this work, the authors report the field emission characteristics of chemically and physically synthesized Copper Phthalocyanine (CuPc) nanostructures such as nanowires, nanotubes and nanotips. The as prepared samples were characterized by X-Ray diffraction (XRD), Ultra Violet Visible Spectrometer (UV-Vis), Fourier Transform Infra-red Spectroscopy (FTIR), and Field Emission Scanning Electron Microscope (FESEM) and Transmission Electron Microscope (TEM). The field emission characteristics were measured in our home designed field emission set up. The registered turn-on field and local field enhancement factor are found to be less than 5 V/μm and greater than 1000 respectively. The field emission behaviour is also stable for 200 minute. The experimental results are further verified by theoretically using by a finite displacement method as implemented in ANSYS Maxwell simulation package. The obtained results strongly indicate CuPc nanostructures to be the potential candidate as an electron emitter for field emission based display device applications.

Keywords: organic semiconductor, phthalocyanine, nanowires, nanotubes, field emission

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Authors: Violina Angelova, Galina Pevicharova

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A comparative research had been carried out to allow us to determine the quantities and the centers of accumulation of Pb, Cu, Zn and Cd in the vegetative and reproductive organs of the sweet potatoes and to ascertain the possibilities for growing them on soils, polluted with heavy metals. The experiments were performed on agricultural fields contaminated by the (1) Non-Ferrous-Metal Works near Plovdiv, (2) Lead and Zinc Complex near Kardjali and (3) a copper smelter near Pirdop, Bulgaria. The soils used in this experiment were characterized by acid, neutral and slightly alkaline reaction, loamy texture and a moderate content of organic matter. The total content of Zn, Pb, and Cd was high and exceeded the limit value in agriculture soils. Sweet potatoes were in a 2-year rotation scheme on three blocks in the experimental field. On reaching commercial ripeness the sweet potatoes were gathered and the contents of heavy metals in their different parts – root, tuber (peel and core), leaves and stems, were determined after microwave mineralization. The quantitative measurements were carried out with inductively coupled plasma atomic emission spectroscopy. The contamination of the sweet potatoes was due mainly to the presence of heavy metals in the soil, which entered the plants through their root system, as well as by diffusion through the peel. Pb, Cu, Zn, and Cd were selectively accumulated in the underground parts of the sweet potatoes, and most of all in the root system and the peel. Heavy metals have an impact on the development and productivity of the sweet potatoes. The high anthropogenic contamination leads to an increased assimilation of heavy metals which reduces the yield and the quality of the production of sweet potatoes, as well as leads to decrease of the absolute dry substance and the quantity of sugars in sweet potatoes. Sweet potatoes could be grown on soils, which are light to medium polluted with lead, zinc, and cadmium, as they do not accumulate these elements. On heavily polluted soils, however, (Pb – 1504 mg/kg, Zn – 3322 mg/kg, Cd – 47 mg/kg) the growing of sweet potatoes is not allowed, as the accumulation of Pb and Cd in the core of the potatoes exceeds the Maximum Acceptable Concentration. Acknowledgment: The authors gratefully acknowledge the financial support by the Bulgarian National Science Fund (Project DFNI DH04/9).

Keywords: heavy metals, polluted soils, sweet potatoes, uptake

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Authors: Deepak Kakde, Steve Howdle, Derek Irvine, Cameron Alexander

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The poor aqueous solubility is one of the major obstacles in the formulation development of many drugs. Around 70% of drugs are poorly soluble in aqueous media. In the last few decades, micelles have emerged as one of the major tools for solubilization of hydrophobic drugs. Micelles are nanosized structures (10-100nm) obtained by self-assembly of amphiphilic molecules into the water. The hydrophobic part of the micelle forms core which is surrounded by a hydrophilic outer shell called corona. These core-shell structures have been used as a drug delivery vehicle for many years. Although, the utility of micelles have been reduced due to the lack of sustainable materials. In the present study, a novel methoxy poly(ethylene glycol)-b-poly(ε-decalactone) (mPEG-b-PεDL) copolymer was synthesized by ring opening polymerization (ROP) of renewable ε-decalactone (ε-DL) monomers on methoxy poly(ethylene glycol) (mPEG) initiator using 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD) as a organocatalyst. All the reactions were conducted in bulk to avoid the use of toxic organic solvents. The copolymer was characterized by nuclear magnetic resonance spectroscopy (NMR), gel permeation chromatography (GPC) and differential scanning calorimetry (DSC).The mPEG-b-PεDL block copolymeric micelles containing indomethacin (IND) were prepared by nanoprecipitation method and evaluated as drug delivery vehicle. The size of the micelles was less than 40nm with narrow polydispersity pattern. TEM image showed uniform distribution of spherical micelles defined by clear surface boundary. The indomethacin loading was 7.4% for copolymer with molecular weight of 13000 and drug/polymer weight ratio of 4/50. The higher drug/polymer ratio decreased the drug loading. The drug release study in PBS (pH7.4) showed a sustained release of drug over a period of 24hr. In conclusion, we have developed a new sustainable polymeric material for IND delivery by combining the green synthetic approach with the use of renewable monomer for sustainable development of polymeric nanomedicine.

Keywords: dopolymer, ε-decalactone, indomethacin, micelles

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Authors: Tooba Aslam, Efthalia Chatzisymeon

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UV-assisted irradiation technologies are well-established for water and wastewater treatment. UVC treatments are widely used at large-scale, while UVA irradiation has more often been applied in combination with a catalyst (e.g. TiO₂ or FeSO₄) in smaller-scale systems. A technical issue of these systems is the formation of fouling on the quartz sleeves that houses the lamps. This fouling can prevent complete irradiation, therefore reducing the efficiency of the process. This paper investigates the effects of operational parameters, such as the type of wastewater, irradiation source, H₂O₂ addition, and water pH on fouling formation and, ultimately, the treatment of municipal wastewater. Batch experiments have been performed at lab-scale while monitoring water quality parameters including: COD, TS, TSS, TDS, temperature, pH, hardness, alkalinity, turbidity, TOC, UV transmission, UV₂₅₄ absorbance, and metal concentrations. The residence time of the wastewater in the reactor was 5 days in order to observe any fouling formation on the quartz surface. Over this period, it was observed that chemical oxygen demand (COD) decreased by 30% and 59% during photolysis (Ultraviolet A) and photo-catalysis (UVA/Fe/H₂O₂), respectively. Higher fouling formation was observed with iron-rich and phosphorous-rich wastewater. The highest rate of fouling was developed with phosphorous-rich wastewater, followed by the iron-rich wastewater. Photo-catalysis (UVA/Fe/H₂O₂) had better removal efficiency than photolysis (UVA). This was attributed to the Photo-Fenton reaction, which was initiated under these operational conditions. Scanning electron microscope (SEM) measurements of fouling formed on the quartz sleeves showed that particles vary in size, shape, and structure; some have more distinct structures and are generally larger and have less compact structure than the others. Energy-dispersive X-ray spectroscopy (EDX) results showed that the major metals present in the fouling cake were iron, phosphorous, and calcium. In conclusion, iron-rich wastewaters are more suitable for UV-assisted treatment since fouling formation on quartz sleeves can be minimized by the formation of oxidizing agents during treatment, such as hydroxyl radicals.

Keywords: advanced oxidation processes, photo-fenton treatment, photo-catalysis, wastewater treatment

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Authors: Virginia Martin Torrejon, Binjie Wu

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Gelatine is a protein biopolymer obtained from the partial hydrolysis of animal tissues which contain collagen, the primary structural component in connective tissue. Gelatine hydrogels have attracted considerable research in recent years as an alternative to synthetic materials due to their outstanding gelling properties, biocompatibility and compostability. Surfactants, such as sodium dodecyl sulfate (SDS), are often used in hydrogels solutions as surface modifiers or solubility enhancers, and their incorporation can influence the hydrogel’s viscoelastic properties and, in turn, its processing and applications. Literature usually focuses on studying the impact of formulation parameters (e.g., gelatine content, gelatine strength, additives incorporation) on gelatine hydrogels properties, but processing parameters, such as curing temperature, are commonly overlooked. For example, some authors have reported a decrease in gel strength at lower curing temperatures, but there is a lack of research on systematic viscoelastic characterisation of high strength gelatine and gelatine-SDS systems at a wide range of curing temperatures. This knowledge is essential to meet and adjust the technological requirements for different applications (e.g., viscosity, setting time, gel strength or melting/gelling temperature). This work investigated the effect of curing temperature (10, 15, 20, 23 and 25 and 30°C) on the elastic modulus (G’) and melting temperature of high strength gelatine-SDS hydrogels, at 10 wt% and 20 wt% gelatine contents, by small-amplitude oscillatory shear rheology coupled with Fourier Transform Infrared Spectroscopy. It also correlates the gel strength obtained by rheological measurements with the gel strength measured by texture analysis. Gelatine and gelatine-SDS hydrogels’ rheological behaviour strongly depended on the curing temperature, and its gel strength and melting temperature can be slightly modified to adjust it to given processing and applications needs. Lower curing temperatures led to gelatine and gelatine-SDS hydrogels with considerably higher storage modulus. However, their melting temperature was lower than those gels cured at higher temperatures and lower gel strength. This effect was more considerable at longer timescales. This behaviour is attributed to the development of thermal-resistant structures in the lower strength gels cured at higher temperatures.

Keywords: gelatine gelation kinetics, gelatine-SDS interactions, gelatine-surfactant hydrogels, melting and gelling temperature of gelatine gels, rheology of gelatine hydrogels

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Authors: Christin Koch, Andreas Winkel, Martin Kahlmeyer, Stefan Böhm

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Due to environmental regulations on greenhouse gas emissions and the depletion of fossil fuels, there is an increasing interest in electric vehicles.To maximize their driving range, batteries with high storage capacities are needed. In most electric cars, rechargeable lithium-ion batteries are used because of their high energy density. However, it has to be taken into account that these batteries generate a large amount of heat during the charge and discharge processes. This leads to a decrease in a lifetime and damage to the battery cells when the temperature exceeds the defined operating range. To ensure an efficient performance of the battery cells, reliable thermal management is required. Currently, the cooling is achieved by heat sinks (e.g., cooling plates) bonded to the battery cells with a thermally conductive adhesive (TCA) that directs the heat away from the components. Especially when large amounts of heat have to be dissipated spontaneously due to peak loads, the principle of heat conduction is not sufficient, so attention must be paid to the mechanism of heat storage. An efficient method to store thermal energy is the use of phase change materials (PCM). Through an isothermal phase change, PCM can briefly absorb or release thermal energy at a constant temperature. If the phase change takes place in the transition from solid to liquid, heat is stored during melting and is released to the ambient during the freezing process upon cooling. The presented work displays the great potential of thermally conductive adhesives filled with microencapsulated PCM to limit peak temperatures in battery systems. The encapsulation of the PCM avoids the effects of aging (e.g., migration) and chemical reactions between the PCM and the adhesive matrix components. In this study, microencapsulation has been carried out by in situ polymerization. The microencapsulated PCM was characterized by FT-IR spectroscopy, and the thermal properties were measured by DSC and laser flash method. The mechanical properties, electrical and thermal conductivity, and adhesive toughness of the TCA/PCM composite were also investigated.

Keywords: phase change material, microencapsulation, adhesive bonding, thermal management

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Authors: Feixiong Chen, Naoufel Haddour, Marie Frenea-Robin, Yves MéRieux, Yann Chevolot, Virginie Monnier

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Neonatal thrombopenia occurs when the mother generates antibodies against her baby’s platelet antigens. It is particularly critical for newborns because it can cause coagulation troubles leading to intracranial hemorrhage. In this case, diagnosis must be done quickly to make platelets transfusion immediately after birth. Before transfusion, platelet antigens must be tested carefully to avoid rejection. The majority of thrombopenia (95 %) are caused by antibodies directed against Human Platelet Antigen 1a (HPA-1a) or 5b (HPA-5b). The common method for antigen platelets detection is polymerase chain reaction allowing for identification of gene sequence. However, it is expensive, time-consuming and requires significant blood volume which is not suitable for newborns. We propose to develop a point-of-care device based on double functionalized magnetic colloids with 1) antibodies specific to antigen platelets and 2) highly sensitive electroactive molecules in order to be detected by an electrochemical microsensor. These magnetic colloids will be used first to isolate platelets from other blood components, then to capture specifically platelets bearing HPA-1a and HPA-5b antigens and finally to attract them close to sensor working electrode for improved electrochemical signal. The expected advantages are an assay time lower than 20 min starting from blood volume smaller than 100 µL. Our functionalization procedure based on amine dendrimers and NHS-ester modification of initial carboxyl colloids will be presented. Functionalization efficiency was evaluated by colorimetric titration of surface chemical groups, zeta potential measurements, infrared spectroscopy, fluorescence scanning and cyclic voltammetry. Our results showed that electroactive molecules and antibodies can be immobilized successfully onto magnetic colloids. Application of a magnetic field onto working electrode increased the detected electrochemical signal. Magnetic colloids were able to capture specific purified antigens extracted from platelets.

Keywords: Magnetic Nanoparticles , Electroactive Molecules, Antibody, Platelet

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Authors: Archana Gupta, Rajesh Kumar

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The chemistry of chalcones has generated intensive scientific studies throughout the world. Especially, interest has been focused on the synthesis and biodynamic activities of chalcones. The blue light transmittance, excellent crystallizability and the two planar rings connected through a conjugated double bond show that chalcone derivatives are superior nonlinear organic compounds. 3-(2-Chloro-6-fluoro¬phen¬yl)-1-(2-thien¬yl) prop-2-en-1-one, 3-(2, 4- Dichlorophenyl) – 1 - (4-methylphenyl) – prop -2-en-1-one, (2E)-3-[4-(methylsulfanyl) phenyl]-1-(4-nitrophenyl) prop-2-en-1-one are some chalcone derivatives exhibiting non linear optical (NLO) properties. NLO materials have been extensively investigated in recent years as they are the key elements for photonic technologies of optical communication, optical interconnect oscillator, amplifier, frequency converter etc. Due to their high molecular hyperpolarizabilities, organic materials display a number of significant NLO properties. Experimental measurements and theoretical calculations on molecular hyperpolarizability β have become one of the key factors in the design of second order NLO materials. Theoretical determination of hyperpolarizability is quite useful both in understanding the relationship between the molecular structure and NLO properties. It also provides a guideline to experimentalists for the design and synthesis of organic NLO materials. Quantum-chemical calculations have made an important contribution to the understanding of the electronic polarization underlying the molecular NLO processes and the establishment of structure–property relationships. In the present investigation, the detailed vibrational analysis of some chalcone derivatives is taken up to understand the correlation of the charge transfer interaction and the NLO activity of the molecules based on density functional theory calculations. The vibrational modes contributing toward the NLO activity have been identified and analyzed. Rather large hyperpolarizability derived by theoretical calculations suggests the possible future use of these compounds for non-linear optical applications. The study suggests the importance of π - conjugated systems for non-linear optical properties and the possibility of charge transfer interactions. We hope that the results of the present study of chalcone derivatives are of assistance in development of new efficient materials for technological applications.

Keywords: hyperpolarizability, molecular structure, NLO material, quantum chemical calculations

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Authors: Alina Muradyan, Lina Babayan, Arsen Nanyan, Gohar Galstyan, Vigen Khachatryan

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We present a photometric method for identifying stars, galaxies and quasars in multi-color surveys, which uses a library of ∼> 65000 color templates for comparison with observed objects. The method aims for extracting the information content of object colors in a statistically correct way, and performs a classification as well as a redshift estimation for galaxies and quasars in a unified approach based on the same probability density functions. For the redshift estimation, we employ an advanced version of the Minimum Error Variance estimator which determines the redshift error from the redshift dependent probability density function itself. The method was originally developed for the Calar Alto Deep Imaging Survey (CADIS), but is now used in a wide variety of survey projects. We checked its performance by spectroscopy of CADIS objects, where the method provides high reliability (6 errors among 151 objects with R < 24), especially for the quasar selection, and redshifts accurate within σz ≈ 0.03 for galaxies and σz ≈ 0.1 for quasars. For an optimization of future survey efforts, a few model surveys are compared, which are designed to use the same total amount of telescope time but different sets of broad-band and medium-band filters. Their performance is investigated by Monte-Carlo simulations as well as by analytic evaluation in terms of classification and redshift estimation. If photon noise were the only error source, broad-band surveys and medium-band surveys should perform equally well, as long as they provide the same spectral coverage. In practice, medium-band surveys show superior performance due to their higher tolerance for calibration errors and cosmic variance. Finally, we discuss the relevance of color calibration and derive important conclusions for the issues of library design and choice of filters. The calibration accuracy poses strong constraints on an accurate classification, which are most critical for surveys with few, broad and deeply exposed filters, but less severe for surveys with many, narrow and less deep filters.

Keywords: VO, ArVO, DFBS, FITS, image processing, data analysis

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Authors: Jyoti Yadav, Rini Singh, Anoop M.D, Nisha Yadav, N. Srinivasa Rao, Fouran Singh, Takayuki Ichikawa, Ankur Jain, Kamlendra Awasthi, Manoj Kumar

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Nanocrystalline films exhibit defects and strain induced by its grain boundaries. Defects and strain affect the physical as well as topological insulating properties of the Bi2Te3 thin films by changing their electronic structure. In the present studies, the effect of Ni7+ ion irradiation on the physical and electrical properties of Bi2Te3 thin films was studied. The films were irradiated at five different fluences (5x1011, 1x1012, 3x1012, 5x1012, 1x1013 ions/cm2). Thin films synthesized using the e-beam technique possess a rhombohedral crystal structure with the R-3m space group. The average crystallite size, as determined by x-ray diffraction (XRD) peak broadening, was found to be 18.5 ± 5 (nm). It was also observed that irradiation increases the induced strain. Raman Spectra of the films demonstrate the splitting of A_1u^1 modes originating from the vibrations along the c-axis. This is by the variation in the lattice parameter ‘c,’ as observed through XRD. The atomic force microscopy study indicates the decrease in surface roughness up to the fluence of 3x1012 ions/cm2 and further increasing the fluence increases the roughness. The decrease in roughness may be due to the growth of smaller nano-crystallites on the surface of thin films due to irradiation-induced annealing. X-ray photoelectron spectroscopy studies reveal the composition to be in close agreement to the nominal values i.e. Bi2Te3. The resistivity v/s temperature measurements revealed an increase in resistivity up to the fluence 3x1012 ions/cm2 and a decrease on further increasing the fluence. The variation in electrical resistivity is corroborated with the change in the carrier concentration as studied through low-temperature Hall measurements. A crossover from the n-type to p-type carriers was achieved in the irradiated films. Interestingly, tuning of the Fermi level by compensating the bulk carriers using ion-irradiation could be achieved.

Keywords: Annealing, Irradiation, Fermi level, Tuning

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Authors: E. Kilicay, Z. Karahaliloglu, B. Hazer, E. B. Denkbas

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In this study, we have prepared concanavaline A (ConA) functionalized curcumin (CUR) loaded PHBHHx (poly(3-hydroxybutyrate-co-3-hydroxyhexanoate)) nanoparticles as a novel and efficient drug delivery system. CUR is a promising anticancer agent for various cancer types. The aim of this study was to evaluate therapeutic potential of curcumin loaded PHBHHx nanoparticles (CUR-NPs) and concanavaline A conjugated curcumin loaded NPs (ConA-CUR NPs) for ovarian cancer treatment. ConA was covalently connected to the carboxylic group of nanoparticles by EDC/NHS activation method. In the ligand attachment experiment, the binding capacity of ConA on the surface of NPs was found about 90%. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analysis showed that the prepared nanoparticles were smooth and spherical in shape. The size and zeta potential of prepared NPs were about 228±5 nm and −21.3 mV respectively. ConA-CUR NPs were characterized by FT-IR spectroscopy which confirmed the existence of CUR and ConA in the nanoparticles. The entrapment and loading efficiencies of different polymer/drug weight ratios, 1/0.125 PHBHHx/CUR= 1.25CUR-NPs; 1/0.25 PHBHHx/CUR= 2.5CUR-NPs; 1/0.5 PHBHHx/CUR= 5CUR-NPs, ConA-1.25CUR NPs, ConA-2.5CUR NPs and ConA-5CUR NPs were found to be ≈ 68%-16.8%; 55%-17.7 %; 45%-33.6%; 70%-15.7%; 60%-17%; 51%-30.2% respectively. In vitro drug release showed that the sustained release of curcumin was observed from CUR-NPs and ConA-CUR NPs over a period of 19 days. After binding of ConA, the release rate was slightly increased due to the migration of curcumin to the surface of the nanoparticles and the matrix integrities was decreased because of the conjugation reaction. This functionalized nanoparticles demonstrated high drug loading capacity, sustained drug release profile, and high and long term anticancer efficacy in human cancer cell lines. Anticancer activity of ConA-CUR NPs was proved by MTT assay and reconfirmed by apoptosis and necrosis assay. The anticancer activity of ConA-CUR NPs was measured in ovarian cancer cells (SKOV-3) and the results revealed that the ConA-CUR NPs had better tumor cells decline activity than free curcumin. The nacked nanoparticles have no cytotoxicity against human ovarian carcinoma cells. Thus the developed functionalized nanoformulation could be a promising candidate in cancer therapy.

Keywords: curcumin, curcumin-PHBHHx nanoparticles, concanavalin A, concanavalin A-curcumin PHBHHx nanoparticles, PHBHHx nanoparticles, ovarian cancer cell

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Authors: Lukasz Kaniuk, Mateusz M. Marzec, Andrzej Bernasik, Urszula Stachewicz

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Electrospinning is one of the commonly used methods to produce micro- or nano-fibers. The properties of electrospun fibers allow them to be used to produce tissue scaffolds, biodegradable bandages, or purification membranes. The morphology of the obtained fibers depends on the composition of the polymer solution as well as the processing parameters. Interesting properties such as high fiber porosity can be achieved by changing humidity during electrospinning. Moreover, by changing voltage polarity in electrospinning, we are able to alternate functional groups at the surface of fibers. In this study, electrospun fibers were made of natural, thermoplastic polyester – PHBV (poly(3-hydroxybutyric acid-co-3-hydrovaleric acid). The fibrous mats were obtained using both positive and negative voltage polarities, and their surface was characterized using X-ray photoelectron spectroscopy (XPS, Ulvac-Phi, Chigasaki, Japan). Furthermore, the effect of the humidity on surface morphology was investigated using scanning electron microscopy (SEM, Merlin Gemini II, Zeiss, Germany). Electrospun PHBV fibers produced with positive and negative voltage polarity had similar morphology and the average fiber diameter, 2.47 ± 0.21 µm and 2.44 ± 0.15 µm, respectively. The change of the voltage polarity had a significant impact on the reorientation of the carbonyl groups what consequently changed the surface potential of the electrospun PHBV fibers. The increase of humidity during electrospinning causes porosity in the surface structure of the fibers. In conclusion, we showed within our studies that the process parameters such as humidity and voltage polarity have a great influence on fiber morphology and chemistry, changing their functionality. Surface properties of polymer fiber have a significant impact on cell integration and attachment, which is very important in tissue engineering. The possibility of changing surface porosity allows the use of fibers in various tissue engineering and drug delivery systems. Acknowledgment: This study was conducted within 'Nanofiber-based sponges for atopic skin treatment' project., carried out within the First TEAM programme of the Foundation for Polish Science co-financed by the European Union under the European Regional Development Fund, project no POIR.04.04.00-00- 4571/18-00.

Keywords: cells integration, electrospun fiber, PHBV, surface characterization

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Authors: Mohamed M. Ibrahim, Gaber A. M. Mersal, Salih Al-Juaid, Samir A. El-Shazly

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A series of mixed ligand complexes, viz., [Cu(BPy)(Gly)X]Y {X = Cl (1), Y = 0; X = 0, Y = ClO4- (2); X = H2O, Y = NO3- (3); X = H2O, Y = CH3COO- (4); and [Cu(BPy)(Gly)-(H2O)]2(SO4) (5) have been synthesized. Their structures and properties were characterized by elemental analysis, thermal analaysis, IR, UV–vis, and ESR spectroscopy, as well as electrochemical measurements including cyclic voltammetry, electrical molar conductivity, and magnetic moment measurements. Complexes 1 and 2 formed slightly distorted square-pyramidal coordination geometries of CuN3OCl and CuN3O2, respectively in which the N,O-donor glycine and N,N-donor bipyridyl bind at the basal plane with chloride ion or water as the axial ligand. Complex 3 shows square planar CuN3O coordination geometry, which exhibits chemically significant hydrogen bonding interactions besides showing coordination polymer formation. The superoxide dismutase and catalase-like activities of all complexes were tested and were found to be promising candidates as durable electron-transfer catalyst being close to the efficiency of the mimicking enzymes displaying either catalase or tyrosinase activity to serve for complete reactive oxygen species (ROS) detoxification, both with respect to superoxide radicals and related peroxides. The DNA binding interaction with super coiled pGEM-T plasmid DNA was investigated by using spectral (absorption and emission) titration and electrochemical techniques. The results revealed that DNA intercalate with complexes 1 and 2 through the groove binding mode. The calculated intrinsic binding constant (Kb) of 1 and 2 were 4.71 and 2.429 × 105 M−1, respectively. Gel electrophoresis study reveals the fact that both complexes cleave super coiled pGEM-T plasmid DNA to nicked and linear forms in the absence of any additives. On the other hand, the interaction of both complexes with DNA, the quasi-reversible CuII/CuI redox couple slightly improves its reversibility with considerable decrease in current intensity. All the experimental results indicate that the bipyridyl mixed copper(II) complex (1) intercalate more effectively into the DNA base pairs.

Keywords: enzyme mimics, mixed ligand complexes, X-ray structures, antioxidant, DNA-binding, DNA cleavage

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Authors: Muhammad Zaman Khan, Vijay Baheti, Jiri Militky

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The present study is focused on the development of multifunctional cotton fabric while having good physiological comfort properties. The functional properties developed include superhydrophobicity (Lotus effect) and UV protection. For this, TiO₂ nanoparticles along with fluorocarbon and organic-inorganic binder have been used to optimize the multifunctional properties. Deposition of TiO₂ nanoparticles with water repellent finish on cotton fabric has been carried out using the pad dry cure method at fix parameters. The morphology and elemental composition of as-deposited particles have been studied by using SEM and EDS. The chemical composition of nanoparticles was determined using energy dispersive spectroscopy. The treated samples exhibited excellent water repellency and UV protection factor. The study of the comfort properties of fabric showed that it had excellent physiological comfort properties. Optimized concentration of water repellent chemical (50g/l) was used in formulations with TiO₂ nanoparticles and organic-inorganic binder. Four formulations were prepared according to the design of the experiment. The formulations were applied to the cotton fabric by roller padding at room temperature (15–20°C). Surface morphology was investigated via SEM images. EDS analysis was also carried out to analyze the composition and atomic percentage of elements. The water contact angle (WCA) of cotton fabric increases with increase in TiO₂ nanoparticles concentration and reaches its maximum value (157°) when the concentration of TiO₂ is 20g/l. The water sliding angle (WSA) decreases and gains minimum value at the same concentration of TiO₂ at which WCA is highest. It was seen samples treated with formulations of TiO₂ nanoparticles exhibits excellent UPF, UV-A and UV-B blocking. However, there was no significant deterioration of air permeability. The water vapor permeability was also slightly decreased (4%) but is acceptable. It can be concluded that there is no significant change in both air and water vapor permeability after nanoparticles coating on the surface of the cotton fabric. The coated cotton fabric has little effect on the stiffness. The stiffness of coated samples was not increased significantly; thus comfort of cotton fabric is not decreased. This functionalized cotton fabric also exhibits good physiological comfort properties. ''The authors are also thankful to student grant competition 21312 provided at Technical University of Liberec''.

Keywords: comfort, functional, nanoparticles, UV protective

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Authors: Imran Khan Swati, Mohammad Younas

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This work aims to explore the potential applications of polymeric hydrophobic membranes and green ionic liquids (ILs). Protic and aprotic ILs were synthesized in the lab., characterized, and tested for CO₂/N₂ and CO₂/CH₄ separation using hydrophobic polymeric membranes via supported ionic liquid membrane (SILM). ILs were verified by FTIR spectroscopy. The SILMs were stable at room temperature up to 0.5 MPa. For CO₂, [BSmim][tos] had the greatest coefficient of solubility and permeability, along with all ILs. At 0.5 MPa, IL [BSmim][tos] was found with a selectivity of 56.2 and 47.5 for pure CO₂/N₂ and CO₂/CH₄, respectively. The ILs synthesized for this study are rated as [BSmim][tos]>[BSmpy][tos]>[Bmim][Cl]>[Bpy][Cl] based on their SILM separation performance. Furthermore, high values of selectivity of [BSmim][tos] and [BSmpy][tos] support the use of ILs for CO₂ separation using SILMs. The study was extended to synthesize and test the ammonium-based ILs, [2-HEA][f] and [2-HEA][Hs]. These ILs achieved 50 % less selectivity for CO₂/N₂ as compared to [BSmim][tos] and [BSmpy][tos]. Nevertheless, the permeability of CO₂ achieved with [2-HEA][f] and [2-HEA][Hs] is more than 20 times higher than the [BSmim][tos] and [BSmpy][tos]. Later, the CO₂/N₂ permeability and selectivity study was extended using a flat sheet membrane contactor with recirculated IL. The contact angle effects, liquid entry pressure (LEP), initial CO₂ concentration, and type of solvents and membrane material on the CO₂ capture efficiency and membrane wetting in the post-combustion capture (PCC) process have been experimentally investigated and evaluated. Polytetrafluoroethylene (PTFE) has shown the most hydrophobic property with 6-170 loss in the contact angle. Furthermore, [Omim][BF4] and [Bmim][BF6] have exhibited only 5-8 % loss in LEP using PTFE membrane support. The CO₂ capture efficiency has been achieved as 80.8-99.8 % in different combinations of ILs and membrane support, keeping all other variables constant. While increasing CO₂ concentration from 15 to 45 % vol., an increase of nearly three folds in the CO₂ mass transfer flux was observed. The combination of [Omim][BF4] and PTFE membrane witnessed good long-term stability with only a 20 % loss in CO₂ capture efficiency in 480 min of continuous operation. A 3- D simulation model for non-dispersive solvent absorption in membrane contactors provides insight into the optimum design of a separation system for a specific application minimizing the overall cost and making the process environment-friendly.

Keywords: Post-combustion CO2 capture, membrane synthesis, process development, permeability and selectivity, ionic liquids

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Authors: Amir Shafiee Kisomi, Mehrdad Mofidi

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Nowadays, fuel cells as a promising alternative for power source have been widely studied owing to their security, high energy density, low operation temperatures, renewable capability and low environmental pollutant emission. The nanoparticles of core-shell type could be widely described in a combination of a shell (outer layer material) and a core (inner material), and their characteristics are greatly conditional on dimensions and composition of the core and shell. In addition, the change in the constituting materials or the ratio of core to the shell can create their special noble characteristics. In this study, a fast technique for the fabrication of a Pd-Co/G/GCE modified electrode is offered. Thermal decomposition reaction of cobalt (II) formate salt over the surface of graphene/glassy carbon electrode (G/GCE) is utilized for the synthesis of Co nanoparticles. The nanoparticles of Pd-Co decorated on the graphene are created based on the following method: (1) Thermal decomposition reaction of cobalt (II) formate salt and (2) the galvanic replacement process Co by Pd2+. The physical and electrochemical performances of the as-prepared Pd-Co/G electrocatalyst are studied by Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Cyclic Voltammetry (CV), and Chronoamperometry (CHA). Galvanic replacement method is utilized as a facile and spontaneous approach for growth of Pd nanostructures. The Pd-Co/G is used as an anode catalyst for ethanol oxidation in alkaline media. The Pd-Co/G not only delivered much higher current density (262.3 mAcm-2) compared to the Pd/C (32.1 mAcm-2) catalyst, but also demonstrated a negative shift of the onset oxidation potential (-0.480 vs -0.460 mV) in the forward sweep. Moreover, the novel Pd-Co/G electrocatalyst represents large electrochemically active surface area (ECSA), lower apparent activation energy (Ea), higher levels of durability and poisoning tolerance compared to the Pd/C catalyst. The paper demonstrates that the catalytic activity and stability of Pd-Co/G electrocatalyst are higher than those of the Pd/C electrocatalyst toward ethanol oxidation in alkaline media.

Keywords: thermal decomposition, nanostructures, galvanic replacement, electrocatalyst, ethanol oxidation, alkaline media

Procedia PDF Downloads 127

Authors: Aditi Taunk, George Iskander, Kitty Ka Kit Ho, Mark Willcox, Naresh Kumar

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Bacterial infections on biomaterial implants and medical devices accounts for 60-70% of all hospital acquired infections (HAIs). Treatment or removal of these infected devices results in high patient mortality and morbidity along with increased hospital expenses. In addition, with no effective strategies currently available and rapid development of antibacterial resistance has made device-related infections extremely difficult to treat. Therefore, in this project we have developed biomaterial surfaces using antibacterial compounds that inhibit biofilm formation by interfering with the bacterial communication mechanism known as quorum sensing (QS). This study focuses on covalent attachment of potent quorum sensing (QS) inhibiting compounds, halogenated furanones (FUs) and dihydropyrrol-2-ones (DHPs), onto glass surfaces. The FUs were attached by photoactivating the azide groups on the surface, and the acid functionalized DHPs were immobilized on amine surface via EDC/NHS coupling. The modified surfaces were tested in vitro against pathogenic organisms such as Staphylococcus aureus and Pseudomonas aeruginosa using confocal laser scanning microscopy (CLSM). Successful attachment of compounds on the substrates was confirmed by X-ray photoelectron spectroscopy (XPS) and contact angle measurements. The antibacterial efficacy was assessed, and significant reduction in bacterial adhesion and biofilm formation was observed on the FU and DHP coated surfaces. The activity of the coating was dependent upon the type of substituent present on the phenyl group of the DHP compound. For example, the ortho-fluorophenyl DHP (DHP-2) exhibited 79% reduction in bacterial adhesion against S. aureus and para-fluorophenyl DHP (DHP-3) exhibited 70% reduction against P. aeruginosa. The results were found to be comparable to DHP coated surfaces prepared in earlier study via Michael addition reaction. FUs and DHPs were able to retain their in vitro antibacterial efficacy after covalent attachment via azide chemistry. This approach is a promising strategy to develop efficient antibacterial biomaterials to reduce device related infections.

Keywords: antibacterial biomaterials, biomedical device-related infections, quorum sensing, surface functionalization

Procedia PDF Downloads 241

Authors: G. Imran, A. Pandurangan

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Epoxides constitute important intermediates for the production of fine and bulk chemicals as well as valuable building blocks for the synthesis of a variety of bioactive molecules. Manganese oxides are used as selective catalyst for various redox type reactions and also effectively used in the field of catalytic disposal of pollutants. Non-toxic, cost efficient factor and more over existence of wide range of oxidation state (+2 to +7) makes catalyst more interesting for both academic research and industrial applications. However, the serious drawback lying is the lower surface area. Exceedingly dispersed manganese oxide grafted over mesoporous solid material KIT-6 through ALD (Atomic Layer Deposition) technique effectively catalyze cyclohexene with H2O2 (30% in water) to corresponding epoxides. Highly selective epoxide >99% with 55.7% conversion of cyclohexene was achieved using huge dispersed active sites of MnOx species containing catalysts. Various weight percent such as (1, 3, 5, 7 & 10 wt %) of manganese (II) acetylacetonate complex was employed as Mn source to post-graft via active silanol groups of KIT-6 and are designated as (Mn-G-KIT-6). XRD, N2 sorption, HR-TEM, DRS-UV-VIS, EPR and H2-TPR were employed for structural and textural properties. Immense Mn species of about 95% proportion on silica matrix obtained was evident from ICP-OES.The resulting materials exhibited Type IV adsorption isotherms indiacting mesopore in nanorange. Si-KIT-6 and Mn-G-KIT-6 materials exhibited surface area of 519-289 m2/g and with decrease in pore volume of 0.96-0.49 cm3/g with pore diameter ranging 7.9- 7.2 with increase in wt%. DRS-UV-VIS spectroscopy and EPR studies reveal that manganese coexists as Mn2+/3+ species as extra-framework sites and frame-work sites that result in dispersion on surface of silica matrix of KIT-6 and incorporated manganese sites with silanol groups along with small sized MnO cluster, evident from HR-TEM which increase with Mn content. Conventional production of epoxides by the intramolecular etherification of chlorohydrins formed by the reaction of alkenes with hypochlorous acid is the major drawbacks obtained recently. The most efficient synthesis of oxiranes (epoxides) is obtained by mesoporous catalysts (Mn-G-KIT-6) are presented here and discussed.

Keywords: ALD, epoxidation, mesoporous, MnOx

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Authors: Grace O. Akinlade, Danjuma D. Maza, Oluwakemi O. Olawolu, Delight O. Babalola, John A. O. Oyekunle, Joshua O. Ojo

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The Mokuro area of Ile-Ife, South West Nigeria, was well known for gold mining in the past (about twenty years ago). However, the place has since been reclaimed and converted to residential area without any environmental risk assessment of the impact of the mining tailings on the environment. Soil, water, and plant samples were collected from 4 different locations around the mine-turned-residential area. Soil samples were pulverized and sieved into finer particles, while the plant samples were dried and pulverized. All the samples were digested and analyzed for As, Pb, Cd, and Zn using atomic absorption spectroscopy (AAS). From the analysis results, the hazard index (HI) was then calculated for the metals. The soil and plant samples were air dried and pulverized, then weighed, after which the samples were packed into special and properly sealed containers to prevent radon gas leakage. After the sealing, the samples were kept for 28 days to attain secular equilibrium. The concentrations of 40K, 238U, and 232Th in the samples were measured using a cesium iodide (CsI) spectrometer and URSA software. The AAS analysis showed that As, Pb, Cd (Toxic metals), and Zn (essential trace metals) are in concentrations lower than permissible limits in plants and soil samples, while the water samples had concentrations higher than permissible limits. The calculated health indices (HI) show that HI for water is >1 and that of plants and soil is <1. Gamma spectrometry result shows high levels of activity concentrations above the recommended limits for all the soil and plant samples collected from the area. Only the water samples have activity concentrations below the recommended limit. Consequently, the absorbed dose, annual effective dose, and excess lifetime cancer risk are all above the recommended safe limit for all the samples except for water samples. In conclusion, all the samples collected from the area are either contaminated with toxic metals or they pose radiological hazards to the consumers. Further detailed study is therefore recommended in order to be able to advise the residents appropriately.

Keywords: toxic metals, gamma spectrometry, Ile-Ife, radiological hazards, gold mining

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Authors: Ariel Vilchez, Francisca Acevedo, Rodrigo Navia

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The wound healing process can be accelerated and improved by the action of antioxidants such as curcumin (Cur) over the tissues; however, the efficacy of curcumin used through the digestive system is not enough to exploit its benefits. Electrospinning presents an alternative to carry curcumin directly to the wounds, and polyhydroxybutyrate (PHB) is proposed as the matrix to load curcumin owing to its biodegradable and biocompatible properties. PHB is among 150 types of Polyhydroxyalkanoates (PHAs) identified, it is a natural thermoplastic polyester produced by microbial fermentation obtained from microorganisms. The proposed objective is to develop electrospun bacterial PHB-based microfibers containing curcumin for possible biomedical applications. Commercial PHB was solved in Chloroform: Dimethylformamide (4:1) to a final concentration of 7% m/V. Curcumin was added to the polymeric solution at 1%, and 7% m/m regarding PHB. The electrospinning equipment (NEU-BM, China) with a rotary collector was used to obtain Cur-PHB fibers at different voltages and flow rate of the polymeric solution considering a distance of 20 cm from the needle to the collector. Scanning electron microscopy (SEM) was used to determine the diameter and morphology of the obtained fibers. Thermal stability was obtained from Thermogravimetric (TGA) analysis, and Fourier Transform Infrared Spectroscopy (FT-IR) was carried out in order to study the chemical bonds and interactions. A preliminary curcumin release to Phosphate Buffer Saline (PBS) pH = 7.4 was obtained in vitro and measured by spectrophotometry. PHB fibers presented an intact chemical composition regarding the original condition (dust) according to FTIR spectra, the diameter fluctuates between 0.761 ± 0.123 and 2.157 ± 0.882 μm, with different qualities according to their morphology. The best fibers in terms of quality and diameter resulted in sample 2 and sample 6, obtained at 0-10kV and 0.5 mL/hr, and 0-10kV and 1.5 mL/hr, respectively. The melting temperature resulted near 178 °C, according to the bibliography. The crystallinity of fibers decreases while curcumin concentration increases for the studied interval. The curcumin release reaches near 14% at 37 °C at 54h in PBS adjusted to a quasi-Fickian Diffusion. We conclude that it is possible to load curcumin in PHB to obtain continuous, homogeneous, and solvent-free microfibers by electrospinning. Between 0% and 7% of curcumin, the crystallinity of fibers decreases as the concentration of curcumin increases. Thus, curcumin enhances the flexibility of the obtained material. HPLC should be used in further analysis of curcumin release.

Keywords: antioxidant, curcumin, polyhydroxybutyrate, wound healing

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Authors: Y. Saylan, F. Yılmaz, A. Denizli

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Rheumatoid arthritis (RA) which is the most common autoimmune disorder of the body's own immune system attacking healthy cells. RA has both articular and systemic effects.Until now romatiod factor (RF) assay is used the most commonly diagnosed RA but it is not specific. Anti-cyclic citrullinated peptide (anti-CCP) antibodies are IgG autoantibodies which recognize citrullinated peptides and offer improved specificity in early diagnosis of RA compared to RF. Anti-CCP antibodies have specificity for the diagnosis of RA from 91 to 98% and the sensitivity rate of 41-68%. Molecularly imprinted polymers (MIP) are materials that are easy to prepare, less expensive, stable have a talent for molecular recognition and also can be manufactured in large quantities with good reproducibility. Molecular recognition-based adsorption techniques have received much attention in several fields because of their high selectivity for target molecules. Quartz crystal microbalance (QCM) is an effective, simple, inexpensive approach mass changes that can be converted into an electrical signal. The applications for specific determination of chemical substances or biomolecules, crystal electrodes, cover by the thin films for bind or adsorption of molecules. In this study, we have focused our attention on combining of molecular imprinting into nanofilms and QCM nanosensor approaches and producing QCM nanosensor for anti-CCP, chosen as a model protein, using anti-CCP imprinted nanofilms. For this aim, anti-CCP imprinted QCM nanosensor was characterized by Fourier transform infrared spectroscopy, atomic force microscopy, contact angle measurements and ellipsometry. The non-imprinted nanosensor was also prepared to evaluate the selectivity of the imprinted nanosensor. Anti-CCP imprinted QCM nanosensor was tested for real-time detection of anti-CCP from aqueous solution. The kinetic and affinity studies were determined by using anti-CCP solutions with different concentrations. The responses related with mass shifts (Δm) and frequency shifts (Δf) were used to evaluate adsorption properties and to calculate binding (Ka) and dissociation (Kd) constants. To show the selectivity of the anti-CCP imprinted QCM nanosensor, competitive adsorption of anti-CCP and IgM was investigated.The results indicate that anti-CCP imprinted QCM nanosensor has a higher adsorption capabilities for anti-CCP than for IgM, due to selective cavities in the polymer structure.

Keywords: anti-CCP, molecular imprinting, nanosensor, rheumatoid arthritis, QCM

Procedia PDF Downloads 335

Authors: Olawale S. Fatoba, Stephen A. Akinlabi, Esther T. Akinlabi, Rezvan Gharehbaghi

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The performance of material surface under wear and corrosion environments cannot be fulfilled by the conventional surface modifications and coatings. Therefore, different industrial sectors need an alternative technique for enhanced surface properties. Titanium and its alloys possess poor tribological properties which limit their use in certain industries. This paper focuses on the effect of hybrid coatings Al-Cu-Fe on a grade five titanium alloy using laser metal deposition (LMD) process. Icosahedral Al-Cu-Fe as quasicrystals is a relatively new class of materials which exhibit unusual atomic structure and useful physical and chemical properties. A 3kW continuous wave ytterbium laser system (YLS) attached to a KUKA robot which controls the movement of the cladding process was utilized for the fabrication of the coatings. The titanium cladded surfaces were investigated for its hardness, corrosion and tribological behaviour at different laser processing conditions. The samples were cut to corrosion coupons, and immersed into 3.65% NaCl solution at 28oC using Electrochemical Impedance Spectroscopy (EIS) and Linear Polarization (LP) techniques. The cross-sectional view of the samples was analysed. It was found that the geometrical properties of the deposits such as width, height and the Heat Affected Zone (HAZ) of each sample remarkably increased with increasing laser power due to the laser-material interaction. It was observed that there are higher number of aluminum and titanium presented in the formation of the composite. The indentation testing reveals that for both scanning speed of 0.8 m/min and 1m/min, the mean hardness value decreases with increasing laser power. The low coefficient of friction, excellent wear resistance and high microhardness were attributed to the formation of hard intermetallic compounds (TiCu, Ti2Cu, Ti3Al, Al3Ti) produced through the in situ metallurgical reactions during the LMD process. The load-bearing capability of the substrate was improved due to the excellent wear resistance of the coatings. The cladded layer showed a uniform crack free surface due to optimized laser process parameters which led to the refinement of the coatings.

Keywords: Al-Cu-Fe coating, corrosion, intermetallics, laser metal deposition, Ti-6Al-4V alloy, wear resistance

Procedia PDF Downloads 145

Authors: Doaa H. Elgohary, Dina M. Hamoda, S. Yahia

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Technical textiles refer to textile materials that are engineered and designed to have specific functionalities and performance characteristics beyond their traditional use as apparel or upholstery fabrics. These textiles are usually developed for their unique properties such as strength, durability, flame retardancy, chemical resistance, waterproofing, insulation and other special properties. The development and use of technical textiles are constantly evolving, driven by advances in materials science, manufacturing technologies and the demand for innovative solutions in various industries. Kevlar 29 is a type of aramid fiber developed by DuPont. It is a high-performance material known for its exceptional strength and resistance to impact, abrasion, and heat. Kevlar 29 belongs to the Kevlar family, which includes different types of aramid fibers. Kevlar 29 is primarily used in applications that require strength and durability, such as ballistic protection, body armor, and body armor for military and law enforcement personnel. It is also used in the aerospace and automotive industries to reinforce composite materials, as well as in various industrial applications. Two different Kevlar samples were used coated with cooper lithium silicate (CLS); ten different mechanical and physical properties (weight, thickness, tensile strength, elongation, stiffness, air permeability, puncture resistance, thermal conductivity, stiffness, and spray test) were conducted to approve its functional performance efficiency. The influence of different mechanical properties was statistically analyzed using an independent t-test with a significant difference at P-value = 0.05. The radar plot was calculated and evaluated to determine the best-performing samples. The results of the independent t-test observed that all variables were significantly affected by yarn counts except water permeability, which has no significant effect. All properties were evaluated for samples 1 and 2, a radar chart was used to determine the best attitude for samples. The radar chart area was calculated, which shows that sample 1 recorded the best performance, followed by sample 2. The surface morphology of all samples and the coating materials was determined using a scanning electron microscope (SEM), also Fourier Transform Infrared Spectroscopy Measurement for the two samples.

Keywords: cooper lithium silicate, independent t-test, kevlar, technical textiles.

Procedia PDF Downloads 46

Authors: Sahar Abbaszadeh, Sharifah Rafidah Wan Alwi, Colin Webb, Nahid Ghasemi, Ida Idayu Muhamad

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Toxic heavy metal discharges into environment due to rapid industrialization is a serious pollution problem that has drawn global attention towards their adverse impacts on both the structure of ecological systems as well as human health. Lead as toxic and bio-accumulating elements through the food chain, is regularly entering to water bodies from discharges of industries such as plating, mining activities, battery manufacture, paint manufacture, etc. The application of conventional methods to degrease and remove Pb(II) ion from wastewater is often restricted due to technical and economic constrains. Therefore, the use of various agro-wastes as low-cost bioadsorbent is found to be attractive since they are abundantly available and cheap. In this study, activated carbon of papaya peel (AC-PP) (as locally available agricultural waste) was employed to evaluate its Pb(II) uptake capacity from single-solute solutions in sets of batch mode experiments. To assess the surface characteristics of the adsorbents, the scanning electron microscope (SEM) coupled with energy disperse X-ray (EDX), and Fourier transform infrared spectroscopy (FT-IR) analysis were utilized. The removal amount of Pb(II) was determined by atomic adsorption spectrometry (AAS). The effects of pH, contact time, the initial concentration of Pb(II) and adsorbent dosage were investigated. The pH value = 5 was observed as optimum solution pH. The optimum initial concentration of Pb(II) in the solution for AC-PP was found to be 200 mg/l where the amount of Pb(II) removed was 36.42 mg/g. At the agitating time of 2 h, the adsorption processes using 100 mg dosage of AC-PP reached equilibrium. The experimental results exhibit high capability and metal affinity of modified papaya peel waste with removal efficiency of 93.22 %. The evaluation results show that the equilibrium adsorption of Pb(II) was best expressed by Freundlich isotherm model (R2 > 0.93). The experimental results confirmed that AC-PP potentially can be employed as an alternative adsorbent for Pb(II) uptake from industrial wastewater for the design of an environmentally friendly yet economical wastewater treatment process.

Keywords: activated carbon, bioadsorption, lead removal, papaya peel, wastewater treatment

Procedia PDF Downloads 258

Authors: Özge Alptoğa, Nuray Uçar, Nilgün Karatepe Yavuz, Ayşen Önen

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Sulfur dioxide (SO₂) is a very toxic air pollutant gas and it causes the greenhouse effect, photochemical smog, and acid rain, which threaten human health severely. Thus, the capture of SO₂ gas is very important for the environment. Graphene which is two-dimensional material has excellent mechanical, chemical, thermal properties, and many application areas such as energy storage devices, gas adsorption, sensing devices, and optical electronics. Further, graphene oxide (GO) is examined as a good adsorbent because of its important features such as functional groups (epoxy, carboxyl and hydroxyl) on the surface and layered structure. The SO₂ adsorption properties of the fibers are usually investigated on carbon fibers. In this study, potential adsorption capacity of GO fibers was researched. GO dispersion was first obtained with Hummers’ method from graphite, and then GO fibers were obtained via wet spinning process. These fibers were converted into a disc shape, dried, and then subjected to SO₂ gas adsorption test. The SO₂ gas adsorption capacity of GO fiber discs was investigated in the fields of utilization of different coagulation baths and reduction by hydrazine hydrate. As coagulation baths, single and triple baths were used. In single bath, only ethanol and CaCl₂ (calcium chloride) salt were added. In triple bath, each bath has a different concentration of water/ethanol and CaCl₂ salt, and the disc obtained from triple bath has been called as reference disk. The fibers which were produced with single bath were flexible and rough, and the analyses show that they had higher SO₂ adsorption capacity than triple bath fibers (reference disk). However, the reduction process did not increase the adsorption capacity, because the SEM images showed that the layers and uniform structure in the fiber form were damaged, and reduction decreased the functional groups which SO₂ will be attached. Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD) analyzes were performed on the fibers and discs, and the effects on the results were interpreted. In the future applications of the study, it is aimed that subjects such as pH and additives will be examined.

Keywords: coagulation bath, graphene oxide fiber, reduction, SO2 gas adsorption

Procedia PDF Downloads 337

Authors: Umar Hayatu Sidik

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Application of liquid base petroleum fuel (petrol and diesel) for transportation fuel causes emissions of greenhouse gases (GHGs), while natural gas (NG) reduces the emissions of greenhouse gases (GHGs). At present, compression and liquefaction are the most matured technology used for transportation system. For transportation use, compression requires high pressure (200–300 bar) while liquefaction is impractical. A relatively low pressure of 30-40 bar is achievable by adsorbed natural gas (ANG) to store nearly compressed natural gas (CNG). In this study, adsorbents for high-pressure adsorption of methane (CH4) was prepared from coconut shells and polyetheretherketone (PEEK) using potassium hydroxide (KOH) and microwave-assisted activation. Design expert software version 7.1.6 was used for optimization and prediction of preparation conditions of the adsorbents for CH₄ adsorption. Effects of microwave power, activation time and quantity of PEEK on the adsorbents performance toward CH₄ adsorption was investigated. The adsorbents were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric (TG) and derivative thermogravimetric (DTG) and scanning electron microscopy (SEM). The ideal CH4 adsorption capacities of adsorbents were determined using volumetric method at pressures of 5, 17, and 35 bar at an ambient temperature and 5 oC respectively. Isotherm and kinetics models were used to validate the experimental results. The optimum preparation conditions were found to be 15 wt% amount of PEEK, 3 minutes activation time and 300 W microwave power. The highest CH4 uptake of 9.7045 mmol CH4 adsorbed/g adsorbent was recorded by M33P15 (300 W of microwave power, 3 min activation time and 15 wt% amount of PEEK) among the sorbents at an ambient temperature and 35 bar. The CH4 equilibrium data is well correlated with Sips, Toth, Freundlich and Langmuir. Isotherms revealed that the Sips isotherm has the best fit, while the kinetics studies revealed that the pseudo-second-order kinetic model best describes the adsorption process. In all scenarios studied, a decrease in temperature led to an increase in adsorption of both gases. The adsorbent (M33P15) maintained its stability even after seven adsorption/desorption cycles. The findings revealed the potential of coconut shell-PEEK as CH₄ adsorbents.

Keywords: adsorption, desorption, activated carbon, coconut shells, polyetheretherketone

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Authors: G. Yakubova, A. Kavetskiy, S. A. Prior, H. A. Torbert

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In-situ soil carbon determination over large soil surface areas (several hectares) is required in regard to carbon sequestration and carbon credit issues. This capability is important for optimizing modern agricultural practices and enhancing soil science knowledge. Collecting and processing representative field soil cores for traditional laboratory chemical analysis is labor-intensive and time-consuming. The neutron-stimulated gamma analysis method can be used for in-situ measurements of primary elements in agricultural soils (e.g., Si, Al, O, C, Fe, and H). This non-destructive method can assess several elements in large soil volumes with no need for sample preparation. Neutron-gamma soil elemental analysis utilizes gamma rays issued from different neutron-nuclei interactions. This process has become possible due to the availability of commercial portable pulse neutron generators, high-efficiency gamma detectors, reliable electronics, and measurement/data processing software complimented by advances in state-of-the-art nuclear physics methods. In Pulsed Fast Thermal Neutron Analysis (PFTNA), soil irradiation is accomplished using a pulsed neutron flux, and gamma spectra acquisition occurs both during and between pulses. This method allows the inelastic neutron scattering (INS) gamma spectrum to be separated from the thermal neutron capture (TNC) spectrum. Based on PFTNA, a mobile system for field-scale soil elemental determinations (primarily carbon) was developed and constructed. Our scanning methodology acquires data that can be directly used for creating soil elemental distribution maps (based on ArcGIS software) in a reasonable timeframe (~20-30 hectares per working day). Created maps are suitable for both agricultural purposes and carbon sequestration estimates. The measurement system design, spectra acquisition process, strategy for acquiring field-scale carbon content data, and mapping of agricultural fields will be discussed.

Keywords: neutron gamma analysis, soil elemental content, carbon sequestration, carbon credit, soil gamma spectroscopy, portable neutron generators, ArcMap mapping

Procedia PDF Downloads 62

Authors: Zh. Saffari, A. Naeimi, M. S. Ekrami-Kakhki, Kh. Khandan-Barani

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The textile industries are becoming a major source of environmental contamination because an alarming amount of dye pollutants are generated during the dyeing processes. Organic dyes are one of the largest pollutants released into wastewater from textile and other industrial processes, which have shown severe impacts on human physiology. Nano-structure compounds have gained importance in this category due their anticipated high surface area and improved reactive sites. In recent years several novel adsorbents have been reported to possess great adsorption potential due to their enhanced adsorptive capacity. Nano-MnO2 has great potential applications in environment protection field and has gained importance in this category because it has a wide variety of structure with large surface area. The diverse structures, chemical properties of manganese oxides are taken advantage of in potential applications such as adsorbents, sensor catalysis and it is also used for wide catalytic applications, such as degradation of dyes. In this study, adsorption of Methyl Violet (MV) dye from aqueous solutions onto MnO2 nanoparticles (MNP) has been investigated. The surface characterization of these nano particles was examined by Particle size analysis, Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and X-Ray Diffraction (XRD). The effects of process parameters such as initial concentration, pH, temperature and contact duration on the adsorption capacities have been evaluated, in which pH has been found to be most effective parameter among all. The data were analyzed using the Langmuir and Freundlich for explaining the equilibrium characteristics of adsorption. And kinetic models like pseudo first- order, second-order model and Elovich equation were utilized to describe the kinetic data. The experimental data were well fitted with Langmuir adsorption isotherm model and pseudo second order kinetic model. The thermodynamic parameters, such as Free energy of adsorption (ΔG°), enthalpy change (ΔH°) and entropy change (ΔS°) were also determined and evaluated.

Keywords: MnO2 nanoparticles, adsorption, methyl violet, isotherm models, kinetic models, surface chemistry

Procedia PDF Downloads 234

Authors: N. Gopal, K. Jaasminerjiit, L. Z. Xiang

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Quinazoline-4(3H)-one ring system has been consistently regarded as promising privileged structural icon owing to its pharmacodynamic versatility in many of its synthetic derivatives as well as in several naturally occurring alkaloids. The literature reveals that 2nd & 3rd positions of the quinazolin-4(3H)-one pharmacophore are the target for substitution with other moieties. On the other hand, sulphanilamide derivatives and isatin moiety also displayed valuable biological activities. Hence, it was thought worthwhile to study the effects of three pharmacophoric moieties like quinazolinone, sulphanilamide and isatin in a single molecule for the better analgesic activity with lower toxicity. Series of novel 2,3-disubstituted quinazolin-4(3H)-one derivatives have been synthesised from the intermediate Schiff base of 2-(4’-substitutedphenyl)-3-[(N-2-oxoindolin-3-ylidene)-4”-sulphonamidophenyl]-quinazolin-4(3H)-one derivatives, which was prepared from reacting 2-(substituted phenyl)-4H-benzo[d][1,3]-oxazin-4-one with sulphanilamide. The required benzoxazinone derivatives were prepared by reacting anthranilic acid with benzoyl chloride. All the compounds structure was characterised by using H1 NMR, IR and Mass spectroscopy. The intermediate Schiff base and final Mannich base compounds were evaluated for their analgesic activity by acetic acid-induced writhing method at the dose of 25mg/kg, 50 mg/kg, and 100 mg/kg (bw) and Diclofenac (25mg/kg of body weight) will be used as the reference drugs. From the results of the study, it has been observed that final Mannich base showed a better analgesic activity when compared to the parent Schiff bases, it was found that compound substituted with N-methyl piperazine at 1st position of the indole nucleus of the final quinazolinone derivatives (GA4B1) i.e. 2-(4’-methoxy phenyl)-3-[4-(N-(1-N-methyl piperazine amine) methyl-2-oxo indoilin-3-ylidene] benzenesulfonyl quinazolin-4(3H)-one increases the analgesic activity and among the synthesised compounds, GA4B1 exhibited quite superior analgesic activity. The remaining Schiff bases and Mannich base derivatives exhibited moderate analgesic activity. All the compounds showed a dose dependent activity. None of the synthesised compound showed ulcer index whereas the standard drug, diclofenac [25 mg/kg (bw)] showed significantly higher gross ulcer index values.

Keywords: analgesic activity, isatin, mannich base, quinazolin-4(3H)-one

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Authors: Mohd Maniruzzaman, Md. Monjurul Alam, Md. Hafezur Rahaman, Anika Amir Mohona

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The consumption of water by various industries is increasing day by day, and the wastewaters from them are increasing as well. These wastewaters consist of various kinds of color, dissolved solids, toxic heavy metals, residual chlorine, and other non-degradable organic materials. If these wastewaters are exposed directly to the environment, it will be hazardous for the environment and personal health. So, it is very necessary to treat these wastewaters before exposing into the environment. In this research, we have demonstrated the successful processing and utilization of fully bio-based cellulose micro crystal (CMC) composite for the removal of heavy metals, dyes, and salinity from industrial wastewaters. Banana rachis micro-cellulose were prepared by acid hydrolysis (H₂SO₄) of banana (Musa acuminata L.) rachis fiber, and Bijoypur raw clay were treated by organic solvent tri-ethyl amine. Composites were prepared with varying different composition of banana rachis nano-cellulose and modified Bijoypur (north-east part in Bangladesh) clay. After the successful characterization of cellulose micro crystal (CMC) and modified clay, our targeted filter was fabricated with different composition of cellulose micro crystal and clay in the locally fabricated packing column with 7.5 cm as thickness of composites fraction. Waste-water was collected from local small textile industries containing basic yellow 2 as dye, lead (II) nitrate [Pb(NO₃)₂] and chromium (III) nitrate [Cr(NO₃)₃] as heavy metals and saline water was collected from Khulna to test the efficiency of banana rachis cellulose micro crystal-clay composite for removing the above impurities. The filtering efficiency of wastewater purification was characterized by Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction (X-RD), thermo gravimetric analysis (TGA), atomic absorption spectrometry (AAS), scanning electron microscopy (SEM) analyses. Finally, our all characterizations data are shown with very high expected results for in industrial application of our fabricated filter.

Keywords: banana rachis, bio-based filter, cellulose micro crystal-clay composite, wastewaters, synthetic dyes, heavy metal, water salinity

Procedia PDF Downloads 97