Search results for: ultra violet-visible rays spectroscopy (UV-VIS)

Authors: Subodh N. Patel, Abhijit Pusty, Manashi Adhikary, Sandip Bhattacharyya

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The steam superheater (SH) is a coil type heat exchanger which is used to produce superheated steam or to convert the wet steam to dry steam (69.6 kg/cm² and 495°C), generated by a boiler. There were two superheaters in the system, SH I and SH II. SH II is a set of tubes that faces the initial interaction with flue gas at high temperature followed by SH I tubes. After a service life of 2100 hours, a tube in the SH II found to be punctured. Dye penetrant test revealed that out of 50 such tubes, 14 more tubes had severe cracks at a similar location. The failure was investigated in detail. The materials and scale were characterized by optical microscope and advance characterization technique. Scale, observed on fracture surface, was characterized under scanning electron microscope and Raman spectroscopy. Stresses acting on the tubes in working condition were analyzed by finite element method software, ANSYS. Cyclic stresses were observed in the simulation at the same prone location due to restriction in expansion of tubes. Based on scale characterization and stress analysis, it was concluded that the tube failed in thermo-mechanical fatigue. Finally, prevention and control measures were taken to avoid such failure in the future.

Keywords: finite element analysis, oxide scale, superheater tube, thermomechanical fatigue

Procedia PDF Downloads 117

Authors: Madhurima Poddar, Vinay Sharma, Shaikh M. Mobin, Rajneesh Misra

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Three 1,8-naphthalimide (NPI) substituted 4,4-difluoroboradiaza-s-indacene (BODIPY) dyads were synthesized via Pd-catalyzed Sonogashira cross-coupling reaction of ethynyl substituted NPI with the meso-, β- and α-halogenated BODIPYs, respectively. The photophysical and electrochemical data reveals considerable electronic communication between the BODIPY and NPI moieties. The electronic absorption spectrum reveals that the substitution of NPI at α position of BODIPY exhibit better electronic communication between the NPI and the BODIPY units. The electronic structures of all the dyads exhibit planar geometries which are in a good correlation with the structures obtained from single crystal X-ray diffraction. The crystal structures of the dyads exhibit interesting supramolecular interactions. The dyads show good cytocompatibility with the potential of multicolor live-cell imaging; making them excellent candidates for biological applications. The work provides an important strategy of screening the substitution pattern at different position of BODIPYs which will be useful for the design of BODIPY based organic molecules for various optoelectronic applications as well as bio-imaging.

Keywords: bio-imaging studies, cross-coupling, cyclic voltammetry, density functional calculations, fluorescence spectra, single crystal XRD, UV/Vis spectroscopy

Procedia PDF Downloads 145

Authors: P. Shrivastava, S. Vijayalakshmi, A. K. Singh, S. Dalai, R. Teotia, P. Sharma, J. Bellare

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This paper focuses on the synthesis and application of nanobioactive glass for bone regeneration studies. Nanobioactive glass has been synthesized by sol gel method having a combination of silicon, calcium and phosphorous in the molar ratio of 75:21:4. The prepared particles were analyzed for surface morphology by FEG SEM and FEG TEM. Physiochemical properties were investigated using ICP AES, FTIR spectroscopy and X-ray diffraction (XRD) techniques. To ascertain their use for therapeutic use, biocompatibility evaluation of the particles was done by performing soaking studies in SBF and in vitro cell culture studies on MG63 cell lines. Cell morphology was observed by FE SEM and phase contrast microscopy. Nanobioactive glasses (NBG) thus prepared were of 30-200 nm in size, which makes them suitable for nano-biomedical applications. The spherical shape of the particles imparts high surface to volume ratio, promoting fast growth of hydroxyapatite (HA), which is the mineral component of bone. As evaluated by in vitro cell culture studies the NBG was found to enhance the surface activation which enhances osteoblast adhesion. This is an essential parameter to improve bone tissue integration, thereby making nanobioactive glass therapeutically suitable for correcting bone defects.

Keywords: biocompatibility, bone tissue engineering, hydroxyapatite, nanobioactive glass

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Authors: Vusumzi E. Pakade, Themba D. Ntuli, Augustine E. Ofomaja

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Macadamia nutshell biosorbents treated in three different methods (raw Macadamia nutshell powder (RMN), acid-treated Macadamia nutshell (ATMN) and base-treated Macadamia nutshell (BTMN)) were investigated for the adsorption of Cr(VI) from aqueous solutions. Fourier transform infrared spectroscopy (FT-IR) spectra of free and Cr(VI)-loaded sorbents as well as thermogravimetric analysis (TGA) revealed that the acid and base treatments modified the surface properties of the sorbents. The optimum conditions for the adsorption of Cr(VI) by sorbents were pH 2, contact time 10 h, adsorbent dosage 0.2 g L-1, and concentration 100 mg L-1. The different treatment methods altered the surface characteristics of the sorbents and produced different maximum binding capacities of 42.5, 40.6 and 37.5 mg g-1 for RMN, ATMN and BTMN, respectively. The data was fitted into the Langmuir, Freundlich, Redlich-Peterson and Sips isotherms. No single model could clearly explain the data perhaps due to the complexity of process taking place. The kinetic modeling results showed that the process of Cr(VI) biosorption with Macadamia sorbents was better described by a process of chemical sorption in pseudo-second order. These results showed that the three treatment methods yielded different surface properties which then influenced adsorption of Cr(VI) differently.

Keywords: biosorption, chromium(VI), isotherms, Macadamia, reduction, treatment

Procedia PDF Downloads 266

Authors: Hai-Hong Gu, Yan-Jun Ai, Zheng Zhou

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Vanadium and titanium are rare metals with superior properties and are important resources in aerospace, aviation, and military. The vanadium/titanium magnetite are mostly ultra-lean ores, and a large number of tailings has been produced in the exploitation process. The tailings are characterized by loose structure, poor nutrient, complex composition and high trace metal contents. Returning green manure has been shown to not only increase plant biomass and soil nutrients but also change the bioavailability of trace metals and the microbial community structure. Fungi play an important role in decomposing organic matter and increasing soil fertility, and the application of organic matter also affects the community structure of fungi. The effects of green manure plants, alfalfa (Medicago sativa L.), returned to the tailings in situ on community structure of fungi, nutrients and bioavailability of trace metals in vanadium/titanium magnetite tailings were investigated in a pot experiment. The results showed that the fungal community diversity and richness were increase after alfalfa green manure returned in situ. The dominant phyla of the fungal community were Ascomycota, Basidiomycota and Ciliophora, especially, the phyla Ciliophora was rare in ordinary soil, but had been found to be the dominant phyla in tailings. Meanwhile, the nutrient properties and various trace metals may shape the microbial communities by affecting the abundance of fungi. It was found that the plant growth was stimulated and the available N and organic C were significantly improved in the vanadium/titanium magnetite tailing with the long-term returning of alfalfa green manure. Moreover, the DTPA-TEA extractable Cd and Zn concentrations in the vanadium/titanium magnetite tailing were reduced by 7.72%~23.8% and 8.02%~24.4%, respectively, compared with those in the non-returning treatment. The above results suggest that the returning of alfalfa green manure could be a potential approach to improve fungal community structure and restore mine tailing ecosystem.

Keywords: fungal community, green manure returning, vanadium/titanium magnet tailings, trace metals

Procedia PDF Downloads 70

Authors: M. Bouhoun Ali, A. Y. Badjah Hadj Ahmed, M. Attou, A. Elias, M. A. Didi

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The extraction of uranium(VI) from aqueous solutions has been investigated using 1-hydroxyhexadecylidene-1,1-diphosphonic acid (HHDPA) and 1-hydroxydodecylidene-1,1-diphosphonic acid (HDDPA), which were synthesized and characterized by elemental analysis and by FT-IR, 1H NMR, 31P NMR spectroscopy. In this paper, we propose a tentative assignment for the shifts of those two ligands and their specific complexes with uranium(VI). We carried out the extraction of uranium(VI) by HHDPA and HDDPA from [carbon tetrachloride + 2-octanol (v/v: 90%/10%)] solutions. Various factors such as contact time, pH, organic/aqueous phase ratio and extractant concentration were considered. The optimum conditions obtained were: contact time= 20 min, organic/aqueous phase ratio = 1, pH value = 3.0 and extractant concentration = 0.3M. The extraction yields are more significant in the case of the HHDPA which is equipped with a hydrocarbon chain, longer than that of the HDDPA. Logarithmic plots of the uranium(VI) distribution ratio vs. pHeq and the extractant concentration showed that the ratio of extractant to extracted uranium(VI) (ligand/metal) is 2:1. The formula of the complex of uranium(VI) with the HHDPA and the DHDPA is UO2(H3L)2 (HHDPA and DHDPA are denoted as H4L). A spectroscopic analysis has showed that coordination of uranium(VI) takes place via oxygen atoms.

Keywords: liquid-liquid extraction, uranium(vi), 1-hydroxyalkylidene-1, 1-diphosphonic acids, hhdpa, hddpa, aqueous solution

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Authors: Shruti Sakarkar, Jega Jegatheesan, Srinivasan Madapusi

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Photocatalytic membranes have shown great potential for the removal of an organic and inorganic pollutant from wastewater as it combines the degradation and antibacterial properties from photocatalysis and physical separation by the membrane in a single unit. Incorporation of the semiconductor in membrane structure results in enhancing the performance and the properties of the membrane. In this study porous ultrafiltration polyvinylidene fluoride (PVDF) membranes with entrapped TiO₂ nanoparticle were prepared by phase inversion method and further used for the degradation of reactive orange 16 (RO16). Prepared photocatalytic membranes were characterized by the scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), contact angle, and atomic force microscope (AFM). The addition of TiO₂ nanopartparticles improves the strength and thermal stability of the membrane. In particular hydrophilicity and permeability increases with the increase of TiO₂ nanoparticles into the membrane. The photocatalytic membrane achieves 80-85% degrdation of RO16. The impact of different parameters such as pH, concentration of photocatalyst, dye concentration and effect of H₂O₂ were analysed. The best conditions for dye degradation were an initial dye concentration of 50 mg/L, with a membrane containing TiO₂ loading of 2wt%. It was observed that in the presence of H₂O₂, degradation increases with increasing H₂O₂ concentration and reached up to 95-98%. The high quality permeates obtained from the photocatalytic membrane can be reused.

Keywords: photocatalytic membrane, TiO₂, PVDF, nanoparticles

Procedia PDF Downloads 164

Authors: Tomilola J. Ajayi, Moses Ollengo, Lukas le Roux, Michael N. Pillay, Richard J. Staples, Shannon M. Biros Werner E. van Zyl

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The formation, characterization, and dye-sensitized solar cell application of nickel(II), zinc(II) and cadmium(II) ferrocenyl dithiophosphonate complexes were investigated. The multidentate monoanionic ligand [S₂PFc(OH)]¯ (L1) was synthesized from the reaction between ferrocenyl Lawesson’s reagent, [FcP(=S)μ-S]₂ (FcLR), (Fc = ferrocenyl) and water. Ligand L1 could potentially coordinate to metal centers through the S, S’ and O donor atoms. The reaction between metal salt precursors and L1 produced a Ni(II) complex of the type [Ni{S₂P(Fc)(OH)}₂] (1) (molar ratio 1:2), a tetranickel (II) complex of the type [Ni₂{S₂OP(Fc)}₂]₂ (2) (molar ratio (1:1), as well as a Zn(II) complex [Zn{S₂P(Fc)(OH)}₂]₂ (3), and a Cd(II) complex [Cd{S₂P(Fc)(OH)}₂]₂ (4). Complexes 1-4 were characterized by 1H and 31P NMR and FT-IR, and complexes 1 and 2 were additionally analysed by X-Ray crystallography. After co-sensitization, the DSSCs were characterized using UV-Vis, cyclic voltammetry, electrochemical impedance spectroscopy, and photovoltaic measurements (I-V curves). Overall finding shows that co-sensitization of our compounds with ruthenium dye N719 resulted in a better overall solar conversion efficiency than only pure N719 dye under the same experimental conditions. In conclusion, we report the first examples of dye-sensitized solar cells (DSSCs) co-sensitized with ferrocenyl dithiophosphonate complexes.

Keywords: dithiophosphonate, dye sensitized solar cell, co-sensitization, solar efficiency

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Authors: S. Yakut, D. Deger, K. Ulutas, D. Bozoglu

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Plasma poly(ethylene oxide) (pPEO) thin films were deposited between Aluminum (Al) electrodes on glass substrates by plasma assisted physical vapor deposition (PAPVD). The deposition was operated inside Argon plasma under 10⁻³ Torr and the thicknesses of samples were determined as 20, 100, 250, 500 nm. The plasma was produced at 5 W by magnetron connected to RF power supply. The capacitance C and dielectric loss factor tan δ were measured by Novovontrol Alpha-A high frequency empedance analyzer at freqquency and temperature intervals of 0,1 Hz and 1MHz, 193-353K, respectively. AC conductivity was derived from these values. AC conductivity results exhibited three different conductivity regions except for 20 nm. These regions can be classified as low, mid and high frequency regions. Low frequency region is observed at around 10 Hz and 300 K while mid frequency region is observed at around 1 kHz and 300 K. The last one, high frequency region, is observed at around 1 kHz and 200 K. There are some coinciding definitions for conduction regions, because these regions shift depending on temperature. Low frequency region behaves as DC-like conductivity while mid and high frequency regions show conductivities corresponding to mechanisms such as classical hopping, tunneling, etc. which are observed for amorphous materials. Unlike other thicknesses, for 20 nm sample low frequency region can not be detected in the investigated freuency range. It is thought that this is arised because of the presence of dead layer behavior.

Keywords: plasma polymers, dead layer, dielectric spectroscopy, AC conductivity

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Authors: Opeyemi Peter Idowu

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Breast cancer is prevalent in northern Nigerian women, most especially in Jos, Plateau State, owing to anthropogenic activities such as solid earth mineral mining as far back as 1904. In this study, atomic absorption spectrometry was used to determine the concentration of eight heavy metals (Cd, As, Cr, Cu, Fe, Pb, Ni, and Zn) in cancerous and non-cancerous breast tissues of Jos Nigerian Women. The levels of heavy metals ranged from 1.08 to 29.34 mg/kg, 0.29 to 10.76 mg/kg, 0.35 to 51.93 mg/kg, 5.15 to 62.93 mg/kg, 11.64 to 51.10 mg/kg, 0.42 to 83.16 mg/kg, 2.08 to 43.07 mg/kg and 1.67 to 71.53 mg/kg for Cd, As, Cr, Cu, Fe, Pb, Ni and Zn respectively. Using MATLAB R2016a, significant differences (tᵥ = 0.0041 - 0.0317) existed between the levels of all the heavy metals in cancerous and non-cancerous breast tissues except Fe. At 0.01 level of significance, a positive significant correlation existed between Pb and Fe, Pb and Cu, Pb and Fe, Ni and Fe, Cr and Pb, as well as Ni and Cr (r = 0.583 – 0.998) in cancerous breast tissues. Using ANOVA, significant differences also occurred in the levels of these heavy metals in cancerous breast tissues (p = 1.910510×10⁻²⁶). The relatively high levels of the cancer-induced heavy metals (Cd, As, Cr, and Pb) compared with control indicated contamination or exposure to heavy metals, which could be the major cause of cancer in these female subjects. This was evidence of contamination as a result of exposure by ingestion, inhalation, or other means to one anthropogenic activity of the other. Therapeutic measures such as gastric lavage, ascorbic acid consumption, and divalent cation treatment are all effective ways to manage heavy metal toxicity in the subjects to lower the risk of breast cancer.

Keywords: breast cancer, heavy metals, spectroscopy, bio-accumulation

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Authors: Rajesh Panda, Jimi Tjong, Sanjay K. Nayak, Mohini M. Sain

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The aim of this manuscript was to evaluate the effect of chemical treatment of sisal fibre on the mechanical and viscoelastic properties of bio based epoxy/fibre composites. The composite samples were manufactured through a vacuum infusion process by adding alkyl phenols from cashew nutshell liquid (CSNL). Changes in the chemical structure of the sisal fibres resulting from the treatments were analyzed by Fourier transform infrared spectroscopy (FTIR). Both alkali and silane treatments produced enhancements in the mechanical properties of sisal fibre bundles. The alkali treatment, when combined with the silane treatment, the mechanical properties of epoxy composites notably improved (13%) in comparison to untreated sisal fibre reinforced composites.This was attributed to an enhanced fibre/matrix interface. The incorporation of CSNL into the sisal/epoxy composite enhanced the fibre-matrix interfacial properties because of the addition of -OH groups to the epoxy matrix. The incorporation of sisal fibre imparts stiffness to the epoxy matrix.

Keywords: phenalkamine, sisal fiber, vacuum infusion, cashew nutshell liquid, cashew nutshell liquid (CSNL)

Procedia PDF Downloads 284

Authors: Eko S. Kunarti, Akhmad Syoufian, Indriana Kartini, Agnes

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Fe₃O₄/SiO₂/TiO₂ nanoparticles have been synthesized and applied as a photocatalyst for the recovery of gold from the mixture of Au(III) and Cu(II) ions. The synthesis was started by the preparation of magnetite (Fe₃O₄) using coprecipitation and sonication methods, followed by SiO₂ coating on magnetite using sol-gel reactions, and then TiO₂ coating using sol-gel process. Characterization was performed by using infrared spectroscopy, X-ray diffraction, transmission electron microscopy methods. Activity of Fe₃O₄/SiO₂/TiO₂ nanoparticles was evaluated as a photocatalyst for recovery of gold through photoreduction of Au(III) ions in Au(III) and Cu(II) ions mixture with a ratio of 1:1, in a closed reactor equipped with UV lamp. The photoreduction yield was represented as a percentage (%) of reduced Au(III) which was calculated by substraction of initial Au(III) concentration by the unreduced one. The unreduced Au(III) was determined by atomic absorption spectrometry. Results showed that the Fe₃O₄/SiO₂/TiO₂ nanoparticles were successfully synthesised with excellent magnetic and photocatalytic properties. The nanoparticles present optimum activity at a pH of 5 under UV irradiation for 120 minutes. At the optimum condition, the Fe₃O₄/SiO₂/TiO₂ nanoparticles could reduce Au³⁺ to Au⁰ 97.24%. In the mixture of Au(III) and Cu(II) ions, the Au(III) ions are more easily reducible than Cu(II) ions with the reduction results of 96.9% and 45.80% for Au(III) and Cu(II) ions, respectively. In addition, the presence of Cu(II) ions has no significant effect on the amount of gold recovered and its reduction reaction rate.

Keywords: Fe₃O₄/SiO₂/TiO₂, photocatalyst, recovery, gold, Au(III) and Cu(II) mixture

Procedia PDF Downloads 274

Authors: D. S. Fardhyanti, M. Megawati, H. Prasetiawan, U. Mediaty

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Currently, fossil fuel is supplying most of world’s energy resources. However, fossil fuel resources are depleted rapidly and require an alternative energy to overcome the increasing of energy demands. Bio-oil is one of a promising alternative renewable energy resources which is converted from biomass through pyrolysis or fast pyrolysis process. Bio-oil is a dark liquid fuel, has a smelling smoke and usually obtained from sugar cane, wood, coconut shell and any other biomass. Sugar cane content analysis showed that the content of oligosaccharide, hemicellulose, cellulose and lignin was 16.69%, 25.66%, 51.27% and 6.38% respectively. Sugar cane is a potential sources for bio-oil production shown by its high content of cellulose. In this study, production of bio-oil from sugar cane bagasse was investigated via fast pyrolysis reactor. Fast pyrolysis was carried out at 500 °C with a heating rate of 10 °C and 1 hour holding time at pyrolysis temperature. Physical properties and chemical composition of bio-oil were analyzed. The viscosity, density, calorific value and molecular weight of produced bio-oil was 3.12 cp, 2.78 g/cm3, 11,048.44 cals/g, and 222.67 respectively. The Bio-oil chemical composition was investigated using GC-MS. Percentage value of furfural, phenol, 3-methyl 1,2-cyclopentanedione, 5-methyl-3-methylene 5-hexen-2-one, 4-methyl phenol, 4-ethyl phenol, 1,2-benzenediol, and 2,6-dimethoxy phenol was 20.76%, 16.42%, 10.86%, 7.54%, 7.05%, 7.72%, 5.27% and 6.79% respectively.

Keywords: bio-oil, pyrolysis, bagasse, sugar cane, gas chromatography-mass spectroscopy

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Authors: Volodymyr Rombakh

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This article was written to substantiate the possibility of detecting the precursors of catastrophic destruction of a structure or device and stopping operation before it. Damage to solids results from breaking the bond between atoms, which requires energy. Modern theories of strength and fracture assume that such energy is due to stress. However, in a letter to W. Thomson (Lord Kelvin) dated December 18, 1856, J.C. Maxwell provided evidence that elastic energy cannot destroy solids. He proposed an equation for estimating a deformable body's energy, equal to the sum of two energies. Due to symmetrical compression, the first term does not change, but the second term is distortion without compression. Both types of energy are represented in the equation as a quadratic function of strain, but Maxwell repeatedly wrote that it is not stress but strain. Furthermore, he notes that the nature of the energy causing the distortion is unknown to him. An article devoted to theories of elasticity was published in 1850. Maxwell tried to express mechanical properties with the help of optics, which became possible only after the creation of quantum mechanics. However, Maxwell's work on elasticity is not cited in the theories of strength and fracture. The authors of these theories and their associates are still trying to describe the phenomena they observe based on classical mechanics. The study of Faraday's experiments, Maxwell's and Rutherford's ideas, made it possible to discover a previously unknown area of electromagnetic radiation. The properties of photons emitted in this reaction are fundamentally different from those of photons emitted in nuclear reactions and are caused by the transition of electrons in an atom. The photons released during all processes in the universe, including from plants and organs in natural conditions; their penetrating power in metal is millions of times greater than that of one of the gamma rays. However, they are not non-invasive. This apparent contradiction is because the chaotic motion of protons is accompanied by the chaotic radiation of photons in time and space. Such photons are not coherent. The energy of a solitary photon is insufficient to break the bond between atoms, one of the stages of which is ionization. The photographs registered the rail deformation by 113 cars, while the Gaiger Counter did not. The author's studies show that the cause of damage to a solid is the breakage of bonds between a finite number of atoms due to the stimulated emission of metastable atoms. The guarantee of the reliability of the structure is the ratio of the energy dissipation rate to the energy accumulation rate, but not the strength, which is not a physical parameter since it cannot be measured or calculated. The possibility of continuous control of this ratio is due to the spontaneous emission of photons by metastable atoms. The article presents calculation examples of the destruction of energy and photographs due to the action of photons emitted during the atomic-proton reaction.

Keywords: atomic-proton reaction, precursors of man-made disasters, strain, stress

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Authors: Subrata Kar, Banani Kundu, Papiya Nandy, Ruma Basu, Sukhen Das

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Natural montmorilollite clay is a common ingredient in pharmaceutical products, both as excipients and active support; hence considered as suitable candidate for Drug Delivery System. In this work, cationic detergent CTAB is used to increase the interlayer spacing of Na+-Montmoriollite clay to intercalate curcumin and methotrexate. Methotrexate is a folic acid antagonist, anti-proliferative and immunosuppressive agent; while curcumin is a bioactive constituent of rhizomes of Curcuma longa, possessing remarkable chemo-preventive and anti-inflammatory properties. The resultant inorganic-organic hybrids are characterized by X-ray diffraction (XRD), Infrared spectroscopy (FTIR) and Thermo Gravimetric Analysis (TGA) to confirm successful intercalation of curcumin and Methotrexate within clay layers. Pharmaceutical investigation of the hybrids is explored by studying the drug loading (%), encapsulation efficiency and release kinetics. Finally in-vitro studies are performed using cancer cells to find the effect of released curcumin to improve the sensitivity of clay bound methotrexate to ameliorate cell death compared to their effectiveness when used without the inorganic aluminosilicate vehicle.

Keywords: montmorillonite, methotrexate, curcumin, loading efficiency, release kinetics, anticancer activity

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Authors: Dionisios Panagiotaras, Dimitrios Papoulis, Elias Stathatos

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Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO2 are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450 °C. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO2 nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties. The composite palygorskite-TiO2 and halloysite-TiO2 films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite -TiO2 or halloysite- TiO2 catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO2 on clay minerals avoiding aggregation.

Keywords: halloysite, palygorskite, photocatalysis, titanium dioxide

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Authors: Wasi Khan, Suboohi Shervani, Swaleha Naseem, Mohd. Shoeb, J. A. Khan, B. R. Singh, A. H. Naqvi

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We have successfully synthesized ZnO/TiO2 nanocomposite using a two-step solochemical synthesis method. The influence of annealing temperature on microstructural, optical, anticandidal, photocatalytic activities and dielectric properties were investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) show the formation of nanocomposite and uniform surface morphology of all samples. The UV-Vis spectra indicate decrease in band gap energy with increase in annealing temperature. The anticandidal activity of ZnO/TiO2 nanocomposite was evaluated against MDR C. albicans 077. The in-vitro killing assay revealed that the ZnO/TiO2 nanocomposite efficiently inhibit the growth of the C. albicans 077. The nanocomposite also exhibited the photocatalytic activity for the degradation of methyl orange as a function of time at 465 nm wavelength. The electrical behaviour of composite has been studied over a wide range of frequencies at room temperature using complex impedance spectroscopy. The dielectric constants, dielectric loss and ac conductivity (σac) were studied as the function of frequency, which have been explained by ‘Maxwell Wagner Model’. The data reveals that the dielectric constant and loss (tanδ) exhibit the normal dielectric behavior and decreases with the increase in frequency.

Keywords: ZnO/TiO2 nanocomposites, SEM, photocatalytic activity, dielectric properties

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Authors: Amir Peyman Soleymani, Jasna Jankovic

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The augmented demand of the clean and renewable energy has necessitated the fuel cell and battery industries to produce more efficient devices at the lower prices, which can be achieved through the improvement of the electrode. Microstructural characterization, as one of the main materials development tools, plays a pivotal role in the production of better clean energy devices. In this study, methods for characterization and studying of the defects and components distribution were performed on the polymer electrolyte membrane fuel cell (PEMFC) and Li-ion battery (LIB) electrodes in 2D and 3D. The particles distribution, porosity, mechanical defects, and component distribution were studied by Scanning Electron Microscope (SEM), SEM-Focused Ion Beam (SEM-FIB), and Scanning Transmission Electron Microscope equipped with Energy Dispersive Spectroscopy (STEM-EDS). The 3D results obtained from X-ray Computed Tomography (XCT) revealed the pathways for electron and ion conductivity and defects progression maps. Computer-aided methods (Avizo) were employed to simulate the properties and performance of the microstructure in the electrodes. The suggestions were provided to improve the performance of PEMFCs and LIBs by adjusting the microstructure and the distribution of the components in the electrodes.

Keywords: PEM fuel cells, Li-ion batteries, 2D and 3D imaging, materials characterizations

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Authors: Dolapop Sribudda, Ura Pancharoen

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The separation of Hg(II) from produced water by hollow fiber contactors (HFC) was investigation. This system included of two hollow fiber modules in the series connecting. The first module used for the extraction reaction and the second module for stripping reaction. Aliquat336 extractant was fed from the organic reservoirs into the shell side of the first hollow fiber module and continuous to the shell side of the second module. The organic liquid was continuously feed recirculate and back to the reservoirs. The feed solution was pumped into the lumen (tube side) of the first hollow fiber module. Simultaneously, the stripping solution was pumped in the same way in tube side of the second module. The feed and stripping solution was fed which had a counter current flow. Samples were kept in the outlet of feed and stripping solution for 1 hour and characterized concentration of Hg(II) by Inductively Couple Plasma Atomic Emission Spectroscopy (ICP-AES). Feed solution was produced water from natural gulf of Thailand. The extractant was Aliquat336 dissolved in kerosene diluent. Stripping solution used was nitric acid (HNO3) and thiourea (NH2CSNH2). The effect of carrier concentration and type of stripping solution were investigated. Results showed that the best condition were 10 % (v/v) Aliquat336 and 1.0 M NH2CSNH2. At the optimum condition, the extraction and stripping of Hg(II) were 98% and 44.2%, respectively.

Keywords: Hg(II), hollow fiber contactor, produced water, wastewater treatment

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Authors: Abhijith N. V., Abhijit Pattnayak, Deepak Kumar

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Nowadays, a group of alloys, namely high entropy alloys (HEA), because of their excellent properties. However, the fabrication of HEAs requires multistage techniques, especially mill-ing, sieving, compaction, sintering, inert media, etc. These processes are laborious, costly, time-oriented, and unsuitable for commercial application. This study adopted a single-stage process-based HVOF thermal spray to develop HEA coating on SS304L substrates. The wear behavior of the deposited HEA coating was explored under different milling time durations (5h, 10h, and 15h, respectively). The effect of feedstock preparation, microstructure, surface chemistry, and mechanical and metallurgical properties on wear resistance was also investigated. The microstructure and composition of both coating and feedstock were evaluated by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis. Finally, the phase distribution was correlated by X-ray diffraction (XRD ) analysis. The results showed that 15h milled powder coating indicated better tribological than the base substrate and 5h,10h milled powder coating. A chemically stable Body Centered Cubic (BCC) solid solution phase was generated within the 15h milled powder-coated system, which resulted in superior tribological properties.

Keywords: high entropy alloys coating, wear mechanism, HVOF coating, microstructure

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Authors: Katie Emerson, Sara Perez-Ojalvo, Jim Komorowski, Danielle Greenberg

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The purpose of this study was to evaluate arginase activity levels in response to combinations of an inositol-stabilized arginine silicate (ASI; Nitrosigine®), L-arginine, and Inositol. Arginine acts as a vasodilator that promotes increased blood flow resulting in enhanced delivery of oxygen and nutrients to the brain and other tissues. ASI alone has been shown to improve performance on cognitive tasks. Arginase, found in human serum, catalyzes the conversion of arginine to ornithine and urea, completing the last step in the urea cycle. Decreasing arginase levels maintains arginine and results in increased nitric oxide production. This study aimed to determine the most effective combination of ASI, L-arginine and inositol for minimizing arginase levels and therefore maximize ASI’s effect on cognition. Serum was taken from untreated healthy donors by separation from clotted factors. Arginase activity of serum in the presence or absence of test products was determined (QuantiChrom™, DARG-100, Bioassay Systems, Hayward CA). The remaining ultra-filtrated serum units were harvested and used as the source for the arginase enzyme. ASI alone or combined with varied levels of Inositol were tested as follows: ASI + inositol at 0.25 g, 0.5 g, 0.75 g, or 1.00 g. L-arginine was also tested as a positive control. All tests elicited changes in arginase activity demonstrating the efficacy of the method used. Adding L-arginine to serum from untreated subjects, with or without inositol only had a mild effect. Adding inositol at all levels reduced arginase activity. Adding 0.5 g to the standardized amount of ASI led to the lowest amount of arginase activity as compared to the 0.25g 0.75g or 1.00g doses of inositol or to L-arginine alone. The outcome of this study demonstrates an interaction of the pairing of inositol with ASI on the activity of the enzyme arginase. We found that neither the maximum nor minimum amount of inositol tested in this study led to maximal arginase inhibition. Since the inhibition of arginase activity is desirable for product formulations looking to maintain arginine levels, the most effective amount of inositol was deemed preferred. Subsequent studies suggest this moderate level of inositol in combination with ASI leads to cognitive improvements including reaction time, executive function, and concentration.

Keywords: arginine, inositol, arginase, cognitive benefits

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Authors: Masek A., Zaborski M.

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In our studies, we propose the use of natural, pro-ecological substances such as polyphenols to protect polymers against ageing. In our studies, we plan to focus on the following compounds: polyphenols, gallic acid esters, flavonoides, carotenoids, curcumin and its derivatives, vitamin A, tocochromanoles, betalain. Phyto-compounds will be selected on the basis of available literature and our preliminary studies. So, we will select compounds with various contents of hydroxyl groups and colored substances capable of participating in color oxidation processes. The natural antioxidants which were added to ethylene-octene elastomer (polyolefin elastomer-Engage) and ethylene-nonbornene (TOPAS). Composites were then subjected to numerous ageing: weathering (climat of Floryda), UV (0,7 W/m2), thermo-oxidation ageing (1000C/10days) and thermal-shock (-600C/+1000C) as a function of the aging time. The efficiency of used anti-ageing agents was checked on the base of the changes after the degradation in deformation energy (tensile strength and elongation at the break), cross-link density, color (parameters L,a,b) and values of carbonyl index (based on the spectrum of infra red spectroscopy), OIT (induction oxygen time as performed in using differential scanning calorimeter -DSC) of the vulcanizates. Therefore polyphenols are considered to be the best stabilisers for polymeric composites against to oxidation processes.

Keywords: polymers, flavonoids, stabilization, ageing, oxidation

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Authors: Seyfullah Madakbas, Emrah Cakmakci

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Polyaniline (PANI), the most studied member of the conductive polymers, has a wide range of uses from several electronic devices to various conductive high-technology applications. Boron nitride (BN) is a boron and nitrogen containing compound with superior chemical and thermal resistance and thermal conductivity. Even though several composites of PANI was prepared in literature, the preparation of h-BN/PANI composites is rare. In this work PANI was polymerized in the presence of different amounts of h-BN (1, 3 and 5% with respect to PANI) by using 0.1 M solution of NH4S2O8 in HCl as the oxidizing agent and conductive composites were prepared. Composites were structurally characterized with FTIR spectroscopy and X-Ray Diffraction (XRD). Thermal properties of conductive composites were determined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric measurements were performed in the frequency range of 106–108 Hz at room temperature. The corresponding bands for the benzenoid and quinoid rings at around 1593 and 1496 cm-1 in the FTIR spectra of the composites proved the formation of polyaniline. Together with the FTIR spectra, XRD analysis also revealed the existence of the interactions between PANI and h-BN. Glass transition temperatures (Tg) of the composites increased with the increasing amount of PANI (from 87 to 101). TGA revealed that the char yield of the composites increased as the amount of h-BN was increased in the composites. Finally the dielectric permittivity of 3 wt.%h-BN-containing composite was measured and found as approximately 17. This work was supported by Marmara University, Commission of Scientific Research Project.

Keywords: dielectric permittivity, h-BN, PANI, thermal analysis

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Authors: Farzad Khajavi

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Studies about the interaction between active pharmaceutical ingredients (API) and excipients are so important in the pre-formulation stage of development of all dosage forms. Analytical techniques such as differential scanning calorimetry (DSC), Thermal gravimetry (TG), and Furrier transform infrared spectroscopy (FTIR) are commonly used tools for investigating regarding compatibility and incompatibility of APIs with excipients. Sometimes the interpretation of data obtained from these techniques is difficult because of severe overlapping of API spectrum with excipients in their mixtures. Principal component analysis (PCA) as a powerful factor analytical method is used in these situations to resolve data matrices acquired from these analytical techniques. Binary mixtures of API and interested excipients are considered and produced. Peaks of FTIR, DSC, or TG of pure API and excipient and their mixtures at different mole ratios will construct the rows of the data matrix. By applying PCA on the data matrix, the number of principal components (PCs) is determined so that it contains the total variance of the data matrix. By plotting PCs or factors obtained from the score of the matrix in two-dimensional spaces if the pure API and its mixture with the excipient at the high amount of API and the 1:1mixture form a separate cluster and the other cluster comprise of the pure excipient and its blend with the API at the high amount of excipient. This confirms the existence of compatibility between API and the interested excipient. Otherwise, the incompatibility will overcome a mixture of API and excipient.

Keywords: API, compatibility, DSC, TG, interactions

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Authors: Niki K. Burns, James R. Pearson, Paul G. Stevenson, Xavier A. Conlan

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In Australian state Victoria, synthetic cannabinoids have recently been made illegal under an amendment to the drugs, poisons and controlled substances act 1981. Identification of synthetic cannabinoids in popular brands of ‘incense’ and ‘potpourri’ has been a difficult and challenging task due to the sample complexity and changes observed in the chemical composition of the cannabinoids of interest. This study has developed analytical methodology for the targeted extraction and determination of synthetic cannabinoids available pre-ban. A simple solvent extraction and solid phase extraction methodology was developed that selectively extracted the cannabinoid of interest. High performance liquid chromatography coupled with UV‐visible and chemiluminescence detection (acidic potassium permanganate and tris (2,2‐bipyridine) ruthenium(III)) were used to interrogate the synthetic cannabinoid products. Mass spectrometry and nuclear magnetic resonance spectroscopy were used for structural elucidation of the synthetic cannabinoids. The tris(2,2‐bipyridine)ruthenium(III) detection was found to offer better sensitivity than the permanganate based reagents. In twelve different brands of herbal incense, cannabinoids were extracted and identified including UR‐144, XLR 11, AM2201, 5‐F‐AKB48 and A796‐260.

Keywords: electrospray mass spectrometry, high performance liquid chromatography, solid phase extraction, synthetic cannabinoids

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Authors: N. Kaneva, A. Bojinova, K. Papazova

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Thin ZnO films are deposited on glass substrates via sol–gel method and dip-coating. The films are prepared from zinc acetate dehydrate as a starting reagent. After that the as-prepared ZnO sol is aged for different periods (0, 1, 3, 5, 10, 15, and 30 days). Nanocrystalline thin films are deposited from various sols. The effect ZnO sols aging time on the structural and photocatalytic properties of the films is studied. The films surface is studied by Scanning Electron Microscopy. The effect of the aging time of the starting solution is studied inrespect to photocatalytic degradation of Reactive Black 5 (RB5) by UV-vis spectroscopy. The experiments are conducted upon UV-light illumination and in complete darkness. The variation of the absorption spectra shows the degradation of RB5 dissolved in water, as a result of the reaction acurring on the surface of the films, and promoted by UV irradiation. The initial concentrations of dye (5, 10 and 20 ppm) and the effect of the aging time are varied during the experiments. The results show, that the increasing aging time of starting solution with respect to ZnO generally promotes photocatalytic activity. The thin films obtained from ZnO sol, which is aged 30 days have best photocatalytic degradation of the dye (97,22%) in comparison with the freshly prepared ones (65,92%). The samples and photocatalytic experimental results are reproducible. Nevertheless, all films exhibit a substantial activity in both UV light and darkness, which is promising for the development of new ZnO photocatalysts by sol-gel method.

Keywords: ZnO thin films, sol-gel, photocatalysis, aging time

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Authors: Reynaldo Esquivel, Pedro Hernandez, Aaron Martinez-Higareda, Sergio Tena-Cano, Enrique Alvarez-Ramos, Armando Lucero-Acuna

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Stimuli-responsive nanomaterials play an essential role in loading, transporting and well-distribution of anti-cancer compounds in the cellular surroundings. The outstanding properties as the Lower Critical Solution Temperature (LCST), hydrolytic cleavage and protonation/deprotonation cycle, govern the release and delivery mechanisms of payloads. In this contribution, we experimentally determine the load efficiency and release of antineoplastic Vincristine Sulfate into PNIPAM-Interpenetrated-Chitosan (PIntC) nanoparticles. Structural analysis was performed by Fourier Transform Infrared Spectroscopy (FT-IR) and Proton Nuclear Magnetic Resonance (1HNMR). ζ-Potential (ζ) and Hydrodynamic diameter (DH) measurements were monitored by Electrophoretic Mobility (EM) and Dynamic Light scattering (DLS) respectively. Mathematical analysis of the release pharmacokinetics reveals a three-phase model above LCST, while a monophasic of Vincristine release model was observed at 32 °C. Cytotoxic essays reveal a noticeable enhancement of Vincristine effectiveness at low drug concentration on HeLa cervix cancer and MDA-MB-231 breast cancer.

Keywords: nanoparticles, vincristine, drug delivery, PNIPAM

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Authors: Abhishek Chandra, Man Singh

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Highly stable and homogeneously dispersed amino acid coated silver nanoparticles (ANP) of ≈ 10 nm diameter, ranging from 420 to 430 nm are prepared on AgNO3 solution addition to gum of Azadirachta indica solution at 373.15 K. The amino acids were selected based on their polarity. The synthesized nanoparticles were characterized by UV-Vis, FTIR spectroscopy, HR-TEM, XRD, SEM and 1H-NMR. The coated nanoparticles were used as catalyst for the reduction of methylene blue dye in presence of Sn(II) in aqueous, anionic and cationic micellar media. The rate of reduction of dye was determined by measuring the absorbance at 660 nm, spectrophotometrically and followed the order: Kcationic > Kanionic > Kwater. After 12 min and in absence of the ANP, only 2%, 3% and 6% of the dye reduction was completed in aqueous, anionic and cationic micellar media respectively while, in presence of ANP coated by polar neutral amino acid with non-polar -R group, the reduction completed to 84%, 95% and 98% respectively. The ANP coated with polar neutral amino acid having non-polar -R group, increased the rate of reduction of the dye by 94, 3205 and 6370 folds in aqueous, anionic and cationic micellar media respectively. Also, the rate of reduction of the dye increased by three folds when the micellar media was changed from anionic to cationic when the ANP is coated by a polar neutral amino acid having a non-polar -R group.

Keywords: silver nanoparticle, surfactant, methylene blue, amino acid

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Authors: Ho-Wa Li, Sai-Wing Tsang

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The excitonic effect in organic semiconductors plays a key role in determining the electronic devices performance. Strong exciton binding energy has been regarded as the detrimental factor limiting the further improvement in organic photovoltaic cells. To the best of our knowledge, only limited reported can be found in measuring the exciton binding energy in organic photovoltaic materials. Conventional sophisticated approach using photoemission spectroscopy (UPS and IPES) would limit the wide access of the investigation. Here, we demonstrate a facile approach to study the electrical and optical quantum efficiencies of a series of conjugated photovoltaic polymer, fullerene and non-fullerene materials. Quantitative values of the exciton binding energy in those prototypical materials were obtained with concise photovoltaic device structure. And the extracted binding energies have excellent agreement with those determined by the conventional photoemission technique. More importantly, our findings can provide valuable information on the excitonic dissociation in the first excited state. Particularly, we find that the high binding energy of some non-fullerene acceptors limits the combination of polymer acceptors for efficiency exciton dissociation. The results bring insight into the engineering of excitonic effect for the development of efficient organic photovoltaic cells.

Keywords: organic photovoltaics, quantum efficiency, exciton binding energy, device physics

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Authors: Chuyi Ye, Minsang Kim, Cheol-Hee Moon

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The organic light emitting diode(OLED), is a potential organic optical functional materials which is considered as the next generation display technology with the advantages such as all-solid state, ultra-thin thickness, active luminous and flexibility. Due to the development of polymer-inorganic substrate, it becomes possible to achieve the flexible OLED display. However the organic light-emitting material is very sensitive to the oxygen and water vapor, and the encapsulation requires water vapor transmission rate(WVTR) and oxygen transmission rate(OTR) as lower as 10-6 g/(m2.d) and 10-5 cm3/(m2.d) respectively. In current situation, the rigorous WVTR and OTR have restricted the application of the OLED display. Traditional epoxy/getter or glass frit approaches, which have been widely applied on glass-substrate-based devices, are not suitable for transparent flexible organic devices, and mechanically flexible thin-film approaches are required. To ensure the OLED’s lifetime, the encapsulation material of the OLED package is very important. In this paper, a low melting point alloy(LMPA)-epoxy mixture in the encapsulation process is introduced. There will be a phase separation when the mixture is heated to the melting of LMPA and the formation of the double line structure between two substrates: the alloy barrier has extremely low WVTR and OTR and the epoxy fills the potential tiny cracks. In our experiment, the PI film is chosen as a flexible transparent substrate, and Mo and Cu are deposited on the PI film successively. Then the two metal layers are photolithographied to the sealing pattern line. The Mo is a transition layer between the PI film and Cu, at the same time, the Cu has a good wettability with the LMPA(Sn-58Bi). At last, pattern is printed with LMPA layer and applied voltage, the gathering Joule heat melt the LMPA and form the double line structure and the OLED package is sealed in the same time. In this research, the double-line encapsulating structure of LMPA and epoxy on the PI film is manufactured for the flexible OLED encapsulation, and in this process it is investigated whether the encapsulation satisfies the requirement of WVTR and OTR for the flexible OLED.

Keywords: encapsulation, flexible, low melting point alloy, OLED

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