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Authors: Venkataraman Sivasankar, Kiyoshi Omine, Hideaki Sano

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The leaching of fluoride from Plaster Board Waste (PBW) is quite feasible in soil and water environments. The Ministry of Environment, Japan recommended the standard limit of 0.8 mgL⁻¹ or less for fluoride. Although the utilization of PBW as a substitute for cement is rather meritorious, its fluoride leaching behavior deteriorates the quality of soil and water and therefore envisaged as a demerit. In view of this fluoride leaching problem, the present research is focused on immobilizing fluoride in PBW. The immobilization experiments were conducted with four chemical systems operated by DAHP (diammonium hydrogen phosphate) and phosphoric acid carbonization of bamboo mass coupled with certain inorganic reactions using reagents such as calcium hydroxide, sodium hydroxide, and aqueous ammonia. The fluoride immobilization was determined after shaking the reactor contents including the plaster board waste for 24 h at 25˚C. In the DAHP system, the immobilization of fluoride was evident from the leaching of fluoride in the range 0.071-0.12 mgL⁻¹, 0.026-0.14 mgL⁻¹ and 0.068-0.12 mgL⁻¹ for the reaction temperatures at 30˚C, 50˚C, and 90˚C, respectively, with final pH of 6.8. The other chemical systems designated as PACCa, PACAm, and PACNa could immobilize fluoride in PBW, and the resulting solution was analyzed with the fluoride less than the Japanese environmental standard of 0.8 mgL⁻¹. In the case of PACAm and PACCa systems, the calcium concentration was found undetectable and witnessed the formation of phosphate compounds. The immobilization of fluoride was found inversely proportional to the increase in the volume of leaching solvent and dose of PBW. Characterization studies of PBW and the solid after fluoride immobilization was done using FTIR (Fourier transform infrared spectroscopy), Raman spectroscopy, FE-SEM ( Field Emission Scanning Electron Microscopy) with EDAX (Energy Dispersive Spectroscopy), XRD (X-ray diffraction), and XPS (X-ray photoelectron spectroscopy). The results revealed the formation of new calcium phosphate compounds such as apatite, monetite, and hydroxylapatite. The participation of such new compounds in fluoride immobilization seems indispensable through the exchange mechanism of hydroxyl and fluoride groups. Acknowledgment: First author thanks to Japanese Society for the Promotion of Science (JSPS) for the award of the fellowship (ID No. 16544).

Keywords: characterization, fluoride, immobilization, plaster board waste

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Authors: Manisha Choudhary, Sudarsan Neogi

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Malachite green (MG), an organic basic dye, has been widely used for the dyeing purpose, as well as a fungicide and antiseptic in aquaculture industry to control fish parasites and disease. However, MG has now turned out to be an extremely controversial compound due to its adverse impact on living beings. Due to high toxicity, proper treatment of wastewater containing MG is utmost important. Among different available technologies, adsorption process is one of the most efficient and cost-effective treatment method due to its simplicity of design, ease of operation and regeneration of used materials. Nonetheless, commercial activated carbon is expensive leading the researchers to focus on utilizing natural resources. In the present work, a species of cactus, Opuntia ficus-indica (OFI), was used to develop a highly efficient, low-cost powdered activated carbon by chemical activation using NaOH. The biosorbent was characterized by Fourier-transform infrared spectroscopy, field emission scanning electron microscope, energy-dispersive X-ray spectroscopy, Brunauer–Emmett–Teller (BET) and X-ray diffraction analysis. Batch adsorption studies were performed to remove MG from an aqueous solution as a function of contact time, initial solution pH, initial dye concentration, biosorbent dosages, the presence of salt and temperature. By increasing the initial dye concentration from 100 to 500 mg/l, adsorption capacity increased from 165.45 to 831.58 mg/g. The adsorption kinetics followed the pseudo-second-order model and the chemisorption mechanisms were revealed. The electrostatic attractions and chemical interactions were observed between amino and hydroxyl groups of the biosorbent and amine groups of the dye. The adsorption was solely controlled by film diffusion. Different isotherm models were used to fit the adsorption data. The excellent recovery of adsorption efficiency after the regeneration of biosorbent indicated the high potential of this adsorbent to remove MG from aqueous solution and an excellent cost-effective biosorbent for wide application in wastewater treatment.

Keywords: adsorption, biosorbent, cactus, malachite green

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Authors: Nikhil Kumar, Asish Bandyopadhyay

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Laser welding process is a capable technology for forming the automobile, microelectronics, marine and aerospace parts etc. In the present work, a mathematical and statistical approach is adopted to study the laser welding of AISI 304 stainless steel. A robotic control 500 W pulsed Nd:YAG laser source with 1064 nm wavelength has been used for welding purpose. Butt joints are made. The effects of welding parameters, namely; laser power, scanning speed and pulse width on the seam width and depth of penetration has been investigated using the empirical models developed by response surface methodology (RSM). Weld quality is directly correlated with the weld geometry. Twenty sets of experiments have been conducted as per central composite design (CCD) design matrix. The second order mathematical model has been developed for predicting the desired responses. The results of ANOVA indicate that the laser power has the most significant effect on responses. Microstructural analysis as well as hardness of the selected weld specimens has been carried out to understand the metallurgical and mechanical behaviour of the weld. Average micro-hardness of the weld is observed to be higher than the base metal. Higher hardness of the weld is the resultant of grain refinement and δ-ferrite formation in the weld structure. The result suggests that the lower line energy generally produce fine grain structure and improved mechanical properties than the high line energy. The combined effects of input parameters on responses have been analyzed with the help of developed 3-D response surface and contour plots. Finally, multi-objective optimization has been conducted for producing weld joint with complete penetration, minimum seam width and acceptable welding profile. Confirmatory tests have been conducted at optimum parametric conditions to validate the applied optimization technique.

Keywords: ANOVA, laser welding, modeling and optimization, response surface methodology

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Authors: Abidullah, Basharat Hussain, Jong Seok Kim

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Polymer electrolyte membrane fuel cell (PEMFC) is an electrochemical cell, which undergoes an oxygen reduction reaction to produce electrical energy. Platinum (Pt) metal has been used as a catalyst since its inception, but expensiveness is the major obstacle in the commercialization of fuel cells. Herein a non-precious group metal (NPGM) is employed instead of Pt to reduce the cost of PEMFCs. Manganese dioxide impregnated carbon nanotubes (MnO₂-CNTs composite) is a catalyst having excellent electrochemical properties and offers a better alternative to the Platinum-based PEMFC. The catalyst is synthesized by impregnating the transition metal on large surface carbonaceous CNTs by hydrothermal synthesis techniques. To enhance the catalytic activity and increase the volumetric current density, the sample was pyrolyzed at 800ᵒC under a nitrogen atmosphere. During pyrolysis, the nitrogen was doped in the framework of CNTs. Then the material was treated with acid for removing the unreacted metals and adding oxygen functional group to the CNT framework. This process ameliorates the catalytic activity of the manganese-based catalyst. The catalyst has been characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and the catalyst activity has been examined by rotating disc electrode (RDE) experiment. The catalyst was strong enough to withstand an austere alkaline environment in experimental conditions and had a high electrocatalytic activity for oxygen reduction reaction (ORR). Linear Sweep Voltammetry (LSV) depicts an excellent current density of -4.0 mA/cm² and an overpotential of -0.3V vs. standard calomel electrode (SCE) in 0.1M KOH electrolyte. Rotating disk electrode (RDE) was conducted at 400, 800, 1200, and 1600 rpm. The catalyst exhibited a higher methanol tolerance and long term durability with respect to commercial Pt/C. The results for MnO₂-CNT show that the low-cost catalyst will supplant the expensive Pt/C catalyst in the fuel cell.

Keywords: carbon nanotubes, methanol fuel cell, oxygen reduction reaction, MnO₂-CNTs

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Authors: Sarre Nzaba, Bulelwa Ntsendwana, Bekkie Mamba, Alex Kuvarega

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The discharge of azo dyes such as Brilliant black (BB) into the water bodies has carcinogenic and mutagenic effects on humankind and the ecosystem. Conventional water treatment techniques fail to degrade these dyes completely thereby posing more problems. Advanced oxidation processes (AOPs) are promising technologies in solving the problem. Anatase type nitrogen-platinum (N, Pt) co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine terminated polyamidoamine generation 1 (PG1) as a template and source of nitrogen. The resultant photocatalysts were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), UV‐Vis diffuse reflectance spectroscopy, photoluminescence spectroscopy (PL), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy (RS), thermal gravimetric analysis (TGA). The results showed that the calcination atmosphere played an important role in the morphology, crystal structure, spectral absorption, oxygen vacancy concentration, and visible light photocatalytic performance of the catalysts. Anatase phase particles ranging between 9- 20 nm were also confirmed by TEM, SEM, and analysis. The origin of the visible light photocatalytic activity was attributed to both the elemental N and Pd dopants and the existence of oxygen vacancies. Co-doping imparted a shift in the visible region of the solar spectrum. The visible light photocatalytic activity of the samples was investigated by monitoring the photocatalytic degradation of brilliant black dye. Co-doped TiO₂ showed greater photocatalytic brilliant black degradation efficiency compared to singly doped N-TiO₂ or Pd-TiO₂ under visible light irradiation. The highest reaction rate constant of 3.132 x 10-2 min⁻¹ was observed for N, Pd co-doped TiO₂ (2% Pd). The results demonstrated that the N, Pd co-doped TiO₂ (2% Pd) sample could completely degrade the dye in 3 h, while the commercial TiO₂ showed the lowest dye degradation efficiency (52.66%).

Keywords: brilliant black, Co-doped TiO₂, polyamidoamine generation 1 (PAMAM G1), photodegradation

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Authors: Farha Mizana Shamsudin, Shahidan Radiman, Yusof Abdullah, Nasri Abdul Hamid

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Oxide dispersion strengthened (ODS) ferritic steels are amongst the most promising candidates for large scale structural materials to be applied in next generation fission and fusion nuclear power reactors. This kind of material is relatively stable at high temperature, possess remarkable mechanical properties and comparatively good resistance from neutron radiation damage. The superior performance of ODS ferritic steels over their conventional properties is attributed to the high number density of nano-sized dispersoids that act as nucleation sites and stable sinks for many small helium bubbles resulting from irradiation, and also as pinning points to dislocation movement and grain growth. ODS ferritic steels are usually produced by powder metallurgical routes involving mechanical alloying (MA) process of Y2O3 and pre-alloyed or elemental metallic powders, and then consolidated by hot isostatic pressing (HIP) or hot extrusion (HE) techniques. In this study, Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (designated as 14YWT) was produced by mechanical alloying process and followed by hot isostatic pressing (HIP) technique. Crystal structure and morphology of this sample were identified and characterized by using X-ray Diffraction (XRD) and field emission scanning electron microscope (FESEM) respectively. The magnetic measurement of this sample at room temperature was carried out by using a vibrating sample magnetometer (VSM). FESEM micrograph revealed a homogeneous microstructure constituted by fine grains of less than 650 nm in size. The ultra-fine dispersoids of size between 5 nm to 19 nm were observed homogeneously distributed within the BCC matrix. The EDS mapping reveals that the dispersoids contain Y-Ti-O nanoclusters and from the magnetization curve plotted by VSM, this sample approaches the behavior of soft ferromagnetic materials. In conclusion, ODS Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (14YWT) ferritic steel was successfully produced by HIP technique in this present study.

Keywords: hot isostatic pressing, magnetization, microstructure, ODS ferritic steel

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Authors: F. Zouai, F. Z. Benabid, S. Bouhelal, D. Benachour

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Nanocomposite polymer / clay are relatively important area of research. These reinforced plastics have attracted considerable attention in scientific and industrial fields because a very small amount of clay can significantly improve the properties of the polymer. The polymeric matrices used in this work are two saturated polyesters ie polyethylene terephthalate (PET) and polyethylene naphthalate (PEN).The success of processing compatible blends, based on poly(ethylene terephthalate) (PET)/ poly(ethylene naphthalene) (PEN)/clay nanocomposites in one step by reactive melt extrusion is described. Untreated clay was first purified and functionalized ‘in situ’ with a compound based on an organic peroxide/ sulfur mixture and (tetramethylthiuram disulfide) as the activator for sulfur. The PET and PEN materials were first separately mixed in the molten state with functionalized clay. The PET/4 wt% clay and PEN/7.5 wt% clay compositions showed total exfoliation. These compositions, denoted nPET and nPEN, respectively, were used to prepare new n(PET/PEN) nanoblends in the same mixing batch. The n(PET/PEN) nanoblends were compared to neat PET/PEN blends. The blends and nanocomposites were characterized using various techniques. Microstructural and nanostructural properties were investigated. Fourier transform infrared spectroscopy (FTIR) results showed that the exfoliation of tetrahedral clay nanolayers is complete and the octahedral structure totally disappears. It was shown that total exfoliation, confirmed by wide angle X-ray scattering (WAXS) measurements, contributes to the enhancement of impact strength and tensile modulus. In addition, WAXS results indicated that all samples are amorphous. The differential scanning calorimetry (DSC) study indicated the occurrence of one glass transition temperature Tg, one crystallization temperature Tc and one melting temperature Tm for every composition. This was evidence that both PET/PEN and nPET/nPEN blends are compatible in the entire range of compositions. In addition, the nPET/nPEN blends showed lower Tc and higher Tm values than the corresponding neat PET/PEN blends. In conclusion, the results obtained indicate that n(PET/PEN) blends are different from the pure ones in nanostructure and physical behavior.

Keywords: blends, exfoliation, DRX, DSC, montmorillonite, nanocomposites, PEN, PET, plastograph, reactive melt-mixing

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Authors: L. Ebralidze, A. Tsertsvadze, D. Berashvili, A. Bakuridze

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Current cancer therapy strategies are based on surgery, radiotherapy and chemotherapy. The problems associated with chemotherapy are one of the biggest challenges for clinical medicine. These include: low specificity, broad spectrum of side effects, toxicity and development of cellular resistance. Therefore, anti-cance drugs need to be develop urgently. Particularly, in order to increase efficiency of anti-cancer drugs and reduce their side effects, scientists work on formulation of nano-drugs. The objective of this study was to develop composition and technology of vincristine nanoparticles using high-molecular carbohydrates of plant origin. Plant polysacharides, particularly, soy bean seed polysaccharides, flaxseed polysaccharides, citrus pectin, gum arabic, sodium alginate were used as objects. Based on biopharmaceutical research, vincristine containing nanoparticle formulations were prepared. High-energy emulsification and solvent evaporation methods were used for preparation of nanosystems. Polysorbat 80, polysorbat 60, sodium dodecyl sulfate, glycerol, polyvinyl alcohol were used in formulation as emulsifying agent and stabilizer of the system. The ratio of API and polysacharides, also the type of the stabilizing and emulsifying agents are very effective on the particle size of the final product. The influence of preparation technology, type and concentration of stabilizing agents on the properties of nanoparticles were evaluated. For the next stage of research, nanosystems were characterized. Physiochemical characterization of nanoparticles: their size, shape, distribution was performed using Atomic force microscope and Scanning electron microscope. The present study explored the possibility of production of NPs using plant polysaccharides. Optimal ratio of active pharmaceutical ingredient and plant polysacharids, the best stabilizer and emulsifying agent was determined. The average range of nanoparticles size and shape was visualized by SEM.

Keywords: nanoparticles, target delivery, natural high molecule carbohydrates, surfactants

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Authors: John Olorunfemi Abe, Olawale Muhammed Popoola, Abimbola Patricia Idowu Popoola

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Hydrogen is an appealing alternative to fossil fuels because of its abundance, low weight, high energy density, and relative lack of contaminants. However, its low density presents a number of storage challenges. Therefore, this work studies the influence of refractory nitride additives consisting of 5 wt. % each of hexagonal boron nitride (h-BN), titanium nitride (TiN), and aluminum nitride (AlN) on hydrogen storage and electrochemical characteristics of Ti6Al4V-based materials produced by spark plasma sintering. The microstructure and phase constituents of the sintered materials were characterized using scanning electron microscopy (in conjunction with energy-dispersive spectroscopy) and X-ray diffraction, respectively. Pressure-composition-temperature (PCT) measurements were used to assess the hydrogen absorption/desorption behavior, kinetics, and storage capacities of the sintered materials, respectively. The pure Ti6Al4V alloy displayed a two-phase (α+β) microstructure, while the modified composites exhibited apparent microstructural modifications with the appearance of nitride-rich secondary phases. It is found that the diffusion process controls the kinetics of the hydrogen absorption. Thus, a faster rate of hydrogen absorption at elevated temperatures ensued. The additives acted as catalysts, lowered the activation energy and accelerated the rate of hydrogen sorption in the composites relative to the monolithic alloy. Ti6Al4V-5 wt. % h-BN appears to be the most promising candidate for hydrogen storage (2.28 wt. %), followed by Ti6Al4V-5 wt. % TiN (2.09 wt. %), whereas Ti6Al4V-5 wt. % AlN shows the least hydrogen storage performance (1.35 wt. %). Accordingly, the developed hydride system (Ti6Al4V-5h-BN) may be competitive for use in applications involving short-range continuous vehicles (~50-100km) as well as stationary applications such as electrochemical devices, large-scale storage cylinders in hydrogen production locations, and hydrogen filling stations.

Keywords: hydrogen storage, Ti6Al4V hydride system, pressure-composition-temperature measurements, refractory nitride additives, spark plasma sintering, Ti6Al4V-based materials

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Authors: Abd El Rahman Mohamed

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Canopic jars made by the ancient Egyptians from different materials were used to preserve the viscera during the mummification process. The canopic jar studied here dates back to the Late Period (712-332 BC). It is found in the Grand Egyptian Museum (GEM), Giza, Egypt. This jar was carved from limestone and covered with a monkey head lid with painted eyes and ears with red pigment and surrounded with black pigment. The jar contains bandages of textile containing mummy viscera with resin and black resin blocks. The canopic jars were made using the sculpting tools that were used by the ancient Egyptians, such as metal chisels (made of copper) and hammers and emptying the mass of the jar from the inside using a tool invented by the ancient Egyptians, which called the emptying drill. This study also aims to use analytical techniques to identify the components of the jar, its contents, pigments, and previous restoration materials and to understand its deterioration aspects. Visual assessment, isolation and identification of fungi, optical microscopy (OM), scanning electron microscopy (SEM), X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) were used in our study. The jar showed different signs of deterioration, such as dust, dirt, stains, scratches, classifications, missing parts, and breaks; previous conservation materials include using iron wire, completion mortar and an adhesive for assembly. The results revealed that the jar was carved from Dolomite Limestone, red Hematite pigment, Mastic resin, and Linen textile bandages. The previous adhesive was Animal Glue and used Gypsum for the previous completion. The most dominant Microbial infection on the jar was found in the fungi of (Penicillium waksmanii), (Nigrospora sphaerica), (Actinomycetes sp) and (Spore-Forming Gram-Positive Bacilli). Conservation procedures have been applied with high accuracy to conserve the jar, including mechanical and chemical cleaning, re-assembling, completion and consolidation.

Keywords: Canopic jar, Consolidation, Mummification, Resin, Viscera.

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Authors: Elmira Solati, Atousa Mehrani, Davoud Dorranian

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Generation of ZnO-Au nanocomposite under laser irradiation of a mixture of the ZnO and Au colloidal suspensions are experimentally investigated. In this work, firstly ZnO and Au nanoparticles are prepared by pulsed laser ablation of the corresponding metals in water using the 1064 nm wavelength of Nd:YAG laser. In a second step, the produced ZnO and Au colloidal suspensions were mixed in different volumetric ratio and irradiated using the second harmonic of a Nd:YAG laser operating at 532 nm wavelength. The changes in the size of the nanostructure and optical properties of the ZnO-Au nanocomposite are studied as a function of the volumetric ratio of ZnO and Au colloidal suspensions. The crystalline structure of the ZnO-Au nanocomposites was analyzed by X-ray diffraction (XRD). The optical properties of the samples were examined at room temperature by a UV-Vis-NIR absorption spectrophotometer. Transmission electron microscopy (TEM) was done by placing a drop of the concentrated suspension on a carbon-coated copper grid. To further confirm the morphology of ZnO-Au nanocomposites, we performed Scanning electron microscopy (SEM) analysis. Room temperature photoluminescence (PL) of the ZnO-Au nanocomposites was measured to characterize the luminescence properties of the ZnO-Au nanocomposites. The ZnO-Au nanocomposites were characterized by Fourier transform infrared (FTIR) spectroscopy. The X-ray diffraction pattern shows that the ZnO-Au nanocomposites had the polycrystalline structure of Au. The behavior observed by images of transmission electron microscope reveals that soldering of Au and ZnO nanoparticles include their adhesion. The plasmon peak in ZnO-Au nanocomposites was red-shifted and broadened in comparison with pure Au nanoparticles. By using the Tauc’s equation, the band gap energy for ZnO-Au nanocomposites is calculated to be 3.15–3.27 eV. In this work, the formation of ZnO-Au nanocomposites shifts the FTIR peak of metal oxide bands to higher wavenumbers. PL spectra of the ZnO-Au nanocomposites show that several weak peaks in the ultraviolet region and several relatively strong peaks in the visible region. SEM image indicates that the morphology of ZnO-Au nanocomposites produced in water was spherical. The TEM images of ZnO-Au nanocomposites demonstrate that with increasing the volumetric ratio of Au colloidal suspension the adhesion increased. According to the size distribution graphs of ZnO-Au nanocomposites with increasing the volumetric ratio of Au colloidal suspension the amount of ZnO-Au nanocomposites with the smaller size is further.

Keywords: Au nanoparticles, pulsed laser ablation, ZnO-Au nanocomposites, ZnO nanoparticles

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Authors: Lucija Pustahija, Christine Bandl, Wolfgang Kern, Christian Mitterer

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Concerning today´s ecological demands, producing reliable materials from sustainable resources is a continuously developing topic. Such an example is the production of carbon materials via pyrolysis of natural gases or biomass. The amazing properties of pyrolytic carbon are utilized in various fields, where in particular the application in building industry is a promising way towards the utilization of pyrolytic carbon and composites based on pyrolytic carbon. For many applications, surface modification of carbon is an important step in tailoring its properties. Therefore, in this paper, an investigation of different oxidation methods was performed to prepare the carbon surface before functionalizing it with organosilanes, which act as coupling agents for epoxy and polyurethane resins. Made in such a way, a building material based on carbon composites could be used as a lightweight, durable material that can be applied where water or air filtration / purification is needed. In this work, both wet and dry oxidation were investigated. Wet oxidation was first performed in solutions of nitric acid (at 120 °C and 150 °C) followed by oxidation in hydrogen peroxide (80 °C) for 3 and 6 h. Moreover, a hydrothermal method (under oxygen gas) in autoclaves was investigated. Dry oxidation was performed under plasma and corona discharges, using different power values to elaborate optimum conditions. Selected samples were then (in preliminary experiments) subjected to a silanization of the surface with amino and glycidoxy organosilanes. The functionalized surfaces were examined by X-ray photon spectroscopy and Fourier transform infrared spectroscopy spectroscopy, and by scanning electron microscopy. The results of wet and dry oxidation methods indicated that the creation of functionalities was influenced by temperature, the concentration of the reagents (and gases) and the duration of the treatment. Sequential oxidation in aq. HNO₃ and H₂O₂ results in a higher content of oxygen functionalities at lower concentrations of oxidizing agents, when compared to oxidizing the carbon with concentrated nitric acid. Plasma oxidation results in non-permanent functionalization on the carbon surface, by which it´s necessary to find adequate parameters of oxidation treatments that could enable longer stability of functionalities. Results of the functionalization of the carbon surfaces with organosilanes will be presented as well.

Keywords: building materials, dry oxidation, organosilanes, pyrolytic carbon, resins, surface functionalization, wet oxidation

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Authors: S. Varnagiris, M. Urbonavicius, S. Tuckute, M. Lelis, K. Bockute

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Amongst many water purification techniques, TiO₂ photocatalysis is recognized as one of the most promising sustainable methods. It is known that for photocatalytical applications anatase is the most suitable TiO₂ phase, however heterojunction of anatase/rutile phases could improve the photocatalytical activity of TiO₂ even further. Despite the relative simplicity of TiO₂ different synthesis methods lead to the highly dispersed crystal phases and photocatalytic activity of the corresponding samples. Accordingly, suggestions and investigations of various innovative methods of TiO₂ synthesis are still needed. In this work structural and photocatalytical properties of TiO₂ films deposited by the unconventional method of simultaneous co-sputtering from two magnetrons powered by pulsed-Direct Current (pDC) and Radio Frequency (RF) power sources with negative bias voltage have been studied. More specifically, TiO₂ film thickness, microstructure, surface roughness, crystal structure, optical transmittance and photocatalytical properties were investigated by profilometer, scanning electron microscope, atomic force microscope, X-ray diffractometer and UV-Vis spectrophotometer respectively. The proposed unconventional two magnetron co-sputtering based TiO₂ film formation method showed very promising results for crystalline TiO₂ film formation while keeping process temperatures below 100 °C. XRD analysis revealed that by using proper combination of power source type and bias voltage various TiO₂ phases (amorphous, anatase, rutile or their mixture) can be synthesized selectively. Moreover, strong dependency between power source type and surface roughness, as well as between the bias voltage and band gap value of TiO₂ films was observed. Interestingly, TiO₂ films deposited by two magnetron co-sputtering without bias voltage had one of the highest band gap values between the investigated films but its photocatalytic activity was superior compared to all other samples. It is suggested that this is due to the dominating nanocrystalline anatase phase with various exposed surfaces including photocatalytically the most active {001}.

Keywords: films, magnetron co-sputtering, photocatalysis, TiO₂

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Authors: Asselah Amel, Affif Chaouche M'yassa, Toudji Amira, Tazerouti Amel

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This study covers two aspects ; the biodegradability and the performances in corrosion inhibition of a series of synthetized surfactants namely Φ- sodium methyl ester sulfonates (Φ-MES: C₁₂-MES, C₁₄-MES and C₁₆-MES. The biodegradability of these organic compounds was studied using the respirometric method, ‘the standard ISO 9408’. Degradation was followed by analysis of dissolved oxygen using the dissolved oxygen meter over 28 days and the results were compared with that of sodium dodecyl sulphate (SDS). The inoculum used consists of activated sludge taken from the aeration basin of the biological wastewater treatment plant in the city of Boumerdes-Algeria. In addition, the anticorrosive performances of Φ-MES surfactants on a carbon steel "X70" were evaluated in an injection water from a well of Hassi R'mel region- Algeria, known as Baremian water, and are compared to sodium dodecyl sulphate. Two technics, the weight loss and the linear polarization resistance corrosion rate (LPR) are used allowing to investigate the relationships between the concentrations of these synthetized surfactants and their surface properties, surface coverage and inhibition efficiency. Various adsorption isotherm models were used to characterize the nature of adsorption and explain their mechanism. The results show that the MES anionic surfactants was readily biodegradable, degrading faster than SDS, about 88% for C₁₂-MES compared to 66% for the SDS. The length of their carbon chain affects their biodegradability; the longer the chain, the lower the biodegradability. The inhibition efficiency of these surfactants is around 78.4% for C₁₂-MES, 76.60% for C₁₄-MES and 98.19% for C₁₆-MES and increases with their concentration and reaches a maximum value around their critical micelle concentrations ( CMCs). Scanning electron microscopy coupled to energy dispersive X-ray spectroscopy allowed to the visualization of a good adhesion of the protective film formed by the surfactants to the surface of the steel. The studied surfactants show the Langmuirian behavior from which the thermodynamic parameters as adsorption constant (Kads), standard free energy of adsorption (〖∆G〗_ads^0 ) are determined. Interaction of the surfactants with steel surface have involved physisorptions.

Keywords: corrosion, surfactants, adsorption, adsorption isotherems

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

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Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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Authors: Mahsa Ahmadi, Mehdi Mehdikhani-Nahrkhalaji, Jaleh Varshosaz, Shadi Farsaei

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Gelatin and hyaluronic acid are commonly used in skin tissue engineering scaffolds, but because of their low mechanical properties and high biodegradation rate, adding a synthetic polymer such as polycaprolactone could improve the scaffold properties. Therefore, we developed a gelatin-hyaluronic acid-polycaprolactone scaffold, containing 0.5 % atorvastatin loaded nanostructured lipid carriers (NLCs) for skin tissue engineering. The atorvastatin loaded NLCs solution was prepared by solvent evaporation method and freeze drying process. Synthesized atorvastatin loaded NLCs was added to the gelatin and hyaluronic acid solution, and a membrane was fabricated with solvent evaporation method. Thereafter it was coated by a thin layer of polycaprolactone via spine coating set. The resulting scaffolds were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analyses. Moreover, mechanical properties, in vitro degradation in 7 days period, and in vitro drug release of scaffolds were also evaluated. SEM images showed the uniform distributed NLCs with an average size of 100 nm in the scaffold structure. Mechanical test indicated that the scaffold had a 70.08 Mpa tensile modulus which was twofold of tensile modulus of normal human skin. A Franz-cell diffusion test was performed to investigate the scaffold drug release in phosphate buffered saline (pH=7.4) medium. Results showed that 72% of atorvastatin was released during 5 days. In vitro degradation test demonstrated that the membrane was degradated approximately 97%. In conclusion, suitable physicochemical and biological properties of membrane indicated that the developed gelatin-hyaluronic acid-polycaprolactone nanocomposite scaffold containing 0.5 % atorvastatin loaded NLCs could be used as a good candidate for skin tissue engineering applications.

Keywords: atorvastatin, gelatin, hyaluronic acid, nano lipid carriers (NLCs), polycaprolactone, skin tissue engineering, solvent casting, solvent evaporation

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Authors: Md. Abdul Aziz

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Sulfide ion is water soluble, highly corrosive, toxic and harmful to the human beings. As a result, knowing the exact concentration of sulfide in water is very important. However, the existing detection and quantification methods have several shortcomings, such as high cost, low sensitivity, and massive instrumentation. Consequently, the development of novel sulfide sensor is relevant. Nevertheless, electrochemical methods gained enormous popularity due to a vast improvement in the technique and instrumentation, portability, low cost, rapid analysis and simplicity of design. Successful field application of electrochemical devices still requires vast improvement, which depends on the physical, chemical and electrochemical aspects of the working electrode. The working electrode made of bulk gold (Au) and platinum (Pt) are quite common, being very robust and endowed with good electrocatalytic properties. High cost, and electrode poisoning, however, have so far hindered their practical application in many industries. To overcome these obstacles, we developed a sulfide sensor based on an indium tin oxide nanoparticle (ITONP)-modified ITO electrode. To prepare ITONP-modified ITO, various methods were tested. Drop-drying of ITONPs (aq.) on aminopropyltrimethoxysilane-functionalized ITO (APTMS/ITO) was found to be the best method on the basis of voltammetric analysis of the sulfide ion. ITONP-modified APTMS/ITO (ITONP/APTMS/ITO) yielded much better electrocatalytic properties toward sulfide electro-οxidation than did bare or APTMS/ITO electrodes. The ITONPs and ITONP-modified ITO were also characterized using transmission electron microscopy and field emission scanning electron microscopy, respectively. Optimization of the type of inert electrolyte and pH yielded an ITONP/APTMS/ITO detector whose amperometrically and chronocoulοmetrically determined limits of detection for sulfide in aqueous solution were 3.0 µM and 0.90 µM, respectively. ITONP/APTMS/ITO electrodes which displayed reproducible performances were highly stable and were not susceptible to interference by common contaminants. Thus, the developed electrode can be considered as a promising tool for sensing sulfide.

Keywords: amperometry, chronocoulometry, electrocatalytic properties, ITO-nanoparticle-modified ITO, sulfide sensor

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Authors: Rachel Fanelwa Ajayi, Anovuyo Jonnas, Emmanuel I. Iwuoha

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Tuberculosis (TB) is an infectious disease caused by the bacterium (Mycobacterium tuberculosis) which has a predilection for lung tissue due to its rich oxygen supply. The mycobacterial cell has a unique innate characteristic which allows it to resist human immune systems and drug treatments; hence, it is one of the most difficult of all bacterial infections to treat, let alone to cure. At the same time, multi-drug resistance TB (MDR-TB) caused by poorly managed TB treatment, is a growing problem and requires the administration of expensive and less effective second line drugs which take much longer treatment duration than fist line drugs. Therefore, to acknowledge the issues of patients falling ill as a result of inappropriate dosing of treatment and inadequate treatment administration, a device with a fast response time coupled with enhanced performance and increased sensitivity is essential. This study involved the synthesis of electroactive platforms for application in the development of nano-biosensors suitable for the appropriate dosing of clinically diagnosed patients by promptly quantifying the levels of the TB drug; Isonaizid. These nano-biosensors systems were developed on gold surfaces using the enzyme N-acetyletransferase 2 coupled to the cysteamine modified poly(8-anilino-1-napthalene sulphonic acid)/zinc oxide nanocomposites. The morphology of ZnO nanoparticles, PANSA/ZnO nano-composite and nano-biosensors platforms were characterized using High-Resolution Transmission Electron Microscopy (HRTEM) and High-Resolution Scanning Electron Microscopy (HRSEM). On the other hand, the elemental composition of the developed nanocomposites and nano-biosensors were studied using Fourier Transform Infra-Red Spectroscopy (FTIR) and Energy Dispersive X-Ray (EDX). The electrochemical studies showed an increase in electron conductivity for the PANSA/ZnO nanocomposite which was an indication that it was suitable as a platform towards biosensor development.

Keywords: N-acetyletransferase 2, isonaizid, tuberculosis, zinc oxide

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Authors: Nivatha Elangovan, Lakshman Neelakantan, Murugaiyan Amirthalingam

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Magnesium and its alloys are widely used for various lightweight engineering and biomedical applications as they render high strength to low weight ratio and excellent corrosion resistance. These alloys possess good bio-compatibility and similar mechanical properties to natural bone. However, manufacturing magnesium alloy components by conventional formative and subtractive methods is challenging due to their poor castability, oxidation potential, and machinability. Therefore, efforts are made to produce complex-design containing magnesium alloy components by additive manufacturing (AM). Arc-wire directed energy deposition (AW-DED), also known as wire arc additive manufacturing (WAAM), is more attractive to produce large volume components with increased productivity than any other AM technique. In this research work, efforts were made to optimise the deposition parameters to build thick-walled (about 10 mm) AZ31 magnesium alloy components by a gas metal arc (GMA) based AW-DED process. By using controlled dip short-circuiting metal transfer in a GMA process, depositions were carried out without defects and spatter formation. Current and voltage waveforms were suitably modified to achieve stable metal transfer. Moreover, the droplet transfer behaviour was analysed using high-speed image analysis and correlated with arc energy. Optical and scanning electron microscopy analyses were carried out to correlate the influence of deposition parameters with the microstructural evolution during deposition. The investigation reveals that by carefully controlling the current-voltage waveform and droplet transfer behaviour, it is possible to stabilise equiaxed grain microstructures in the deposited AZ31 components. The printed component exhibited an improved mechanical property as equiaxed grains improve the ductility and enhance the toughness. The equiaxed grains in the component improved the corrosion-resistant behaviour of other conventionally manufactured components.

Keywords: arc wire directed energy deposition, AZ31 magnesium alloy, equiaxed grain, corrosion

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Authors: Navah Z. Ratzon, Anat Keren, Shlomit Y. Greenberg

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Car accidents are a problem worldwide. Adolescents’ involvement in car accidents is higher in comparison to the overall driving population. Researchers estimate the risk of accidents among adolescents with symptoms of attention-deficit/hyperactivity disorder (ADHD) to be 1.2 to 4 times higher than that of their peers. Individuals with ADHD exhibit unique patterns of eye movements and attentional shifts that play an important role in driving. In addition, deficiencies in cognitive and executive functions among adolescents with ADHD is likely to put them at greater risk for car accidents. Fifteen adolescents with ADHD and 17 matched controls participated in the study. Individuals from both groups attended local public schools and did not have a driver’s license. Participants’ mean age was 16.1 (SD=.23). As part of the experiment, they all completed a driving simulation session, while their eye movements were monitored. Data were recorded by an eye tracker: The entire driving session was recorded, registering the tester’s exact gaze position directly on the screen. Eye movements and simulator data were analyzed using Matlab (Mathworks, USA). Participants’ cognitive and metacognitive abilities were evaluated as well. No correlation was found between saccade properties, regions of interest, and simulator performance in either group, although participants with ADHD allocated more visual scan time (25%, SD = .13%) to a smaller segment of dashboard area, whereas controls scanned the monitor more evenly (15%, SD = .05%). The visual scan pattern found among participants with ADHD indicates a distinct pattern of engagement-disengagement of spatial attention compared to that of non-ADHD participants as well as lower attention flexibility, which likely affects driving. Additionally the lower the results on the cognitive tests, the worse driving performance was. None of the participants had prior driving experience, yet participants with ADHD distinctly demonstrated difficulties in scanning their surroundings, which may impair driving. This stresses the need to consider intervention programs, before driving lessons begin, to help adolescents with ADHD acquire proper driving habits, avoid typical driving errors, and achieve safer driving.

Keywords: ADHD, attentional shifting, driving simulator, eye movements

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Authors: Marine Reymond, Michael Descostes, Marie Muguet, Clemence Besancon, Martine Leermakers, Catherine Beaucaire, Sophie Billon, Patricia Patrier

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²²⁶Ra is one of the radionuclides resulting from the disintegration of ²³⁸U. Due to its half-life (1600 y) and its high specific activity (3.7 x 1010 Bq/g), ²²⁶Ra is found at the ultra-trace level in the natural environment (usually below 1 Bq/L, i.e. 10-13 mol/L). Because of its decay in ²²²Rn, a radioactive gas with a shorter half-life (3.8 days) which is difficult to control and dangerous for humans when inhaled, ²²⁶Ra is subject to a dedicated monitoring in surface waters especially in the context of uranium mining. In natural waters, radionuclides occur in dissolved, colloidal or particular forms. Due to the size of colloids, generally ranging between 1 nm and 1 µm and their high specific surface areas, the colloidal fraction could be involved in the transport of trace elements, including radionuclides in the environment. The colloidal fraction is not always easy to determine and few existing studies focus on ²²⁶Ra. In the present study, a complete multidisciplinary approach is proposed to assess the colloidal transport of ²²⁶Ra. It includes water sampling by conventional filtration (0.2µm) and the innovative Diffusive Gradient in Thin Films technique to measure the dissolved fraction (<10nm), from which the colloidal fraction could be estimated. Suspended matter in these waters were also sampled and characterized mineralogically by X-Ray Diffraction, infrared spectroscopy and scanning electron microscopy. All of these data, which were acquired on a rehabilitated former uranium mine, allowed to build a geochemical model using the geochemical calculation code PhreeqC to describe, as accurately as possible, the colloidal transport of ²²⁶Ra. Colloidal transport of ²²⁶Ra was found, for some of the sampling points, to account for up to 95% of the total ²²⁶Ra measured in water. Mineralogical characterization and associated geochemical modelling highlight the role of barite, a barium sulfate mineral well known to trap ²²⁶Ra into its structure. Barite was shown to be responsible for the colloidal ²²⁶Ra fraction despite the presence of kaolinite and ferrihydrite, which are also known to retain ²²⁶Ra by sorption.

Keywords: colloids, mining context, radium, transport

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Authors: Simone F. Medeiros, Jessica M. Fonseca, Gizelda M. Alves, Danilo M. Santos, Sérgio P. Campana-Filho, Amilton M. Santos

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Stimuli responsive and biocompatible hydrogel nanoparticles have gained special attention as systems for potential applications in controlled release of drugs to improve their therapeutic efficacy while minimizing side effects. In this work, novel solid dispersions based on thermo- and pH-responsive poly(N-vinylcaprolactam-co-itaconic acid-co-ethylene- glycol dimethacrylate) hydrogel nanoparticles embedded in chitosan matrices were prepared via spray drying for controlled release of ketoprofen. Firstly, the hydrogel nanoparticles containing ketoprofen were prepared via precipitation polymerization and their stimuli-responsive behavior, thermal properties, chemical composition, encapsulation efficiency and morphology were characterized. Then, hydrogel nanoparticles with different particles size were embedded into chitosan matrices via spray-drying. Scanning electron microscopy (SEM) analyses were performed to investigate the particles size, dispersity and morphology. Finally, ketoprofen release profiles were studied as a function of pH and temperature. Chitosan/poly(NVCL-co-IA-co-EGDMA)-ketoprofen microparticles presented spherical shape, rough surface and pronounced agglomeration, indicating that hydrogels nanoparticles loaded with ketoprofen modified the surface of chitosan matrix. The maximum encapsulation efficiency of ketoprofen into hydrogel nanoparticles was 57.8% and the electrostatic interactions between amino groups from chitosan and carboxylic groups from hydrogel nanoparticles were able to control ketoprofen release. The hydrogel nanoparticles themselves were capable to retard the release of ketoprofen-loaded until 48h of in vitro release tests, while their incorporation into chitosan matrix achieved a maximum percentage of drug release of 45%, using a mass ratio of chitosan: poly(NVCL-co-IA-co-EGDMA equal to 10:7, and 69%, using a mass ratio of chitosan: poly(NVCL-co-IA-co-EGDMA equal to 5:2.

Keywords: hydrogel nanoparticles, poly(N-vinylcaprolactam-co-itaconic acid-co-ethylene- glycol dimethacrylate), chitosan, ketoprofen, spray-drying

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Authors: N. Stevulova, I. Schwarzova, V. Hospodarova, J. Junak, J. Briancin

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Sustainability is becoming a priority for developers and the use of environmentally friendly materials is increasing. Nowadays, the application of raw materials from renewable sources to building materials has gained a significant interest in this research area. Lignocellulosic aggregates and cellulosic fibers are coming from many different sources such as wood, plants and waste. They are promising alternative materials to replace synthetic, glass and asbestos fibers as reinforcement in inorganic matrix of composites. Natural fibers are renewable resources so their cost is relatively low in comparison to synthetic fibers. With the consideration of environmental consciousness, natural fibers are biodegradable so their using can reduce CO₂ emissions in the building materials production. The use of cellulosic fibers in cementitious matrices have gained importance because they make the composites lighter at high fiber content, they have comparable cost - performance ratios to similar building materials and they could be processed from waste paper, thus expanding the opportunities for waste utilization in cementitious materials. The main objective of this work is to find out the possibility of using different wastes: hemp hurds as waste of hemp stem processing and recycled fibers obtained from waste paper for making cement composite products such as mortars based on cellulose fibers. This material was made of cement mortar containing organic filler based on hemp hurds and recycled waste paper. In addition, the effects of fibers and their contents on some selected physical and mechanical properties of the fiber-cement plaster composites have been investigated. In this research organic material have used to mortars as 2.0, 5.0 and 10.0 % replacement of cement weight. Reference sample is made for comparison of physical and mechanical properties of cement composites based on recycled cellulosic fibers and lignocellulosic aggregates. The prepared specimens were tested after 28 days of curing in order to investigate density, compressive strength and water absorbability. Scanning Electron Microscopy examination was also carried out.

Keywords: Hemp hurds, organic filler, recycled paper, sustainable building materials

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Authors: Muhammad Ather Nadeem, Bilal Ahmad Khan, Tasawer Abbas

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Nanoherbicides utilize nanotechnology to enhance the delivery of biological or chemical herbicides using combinations of nanomaterials. The aim of this research was to examine the efficacy of chitosan nanoparticles containing MCPA herbicide as a potential eco-friendly alternative for weed control in wheat crops. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and ultraviolet absorbance were used to analyze the developed nanoparticles. The SEM analysis indicated that the average size of the particles was 35 nm, forming clusters with a porous structure. Both nanoparticles of fluroxyper + MCPA exhibited maximal absorption peaks at a wavelength of 320 nm. The compound fluroxyper +MCPA has a strong peak at a 2θ value of 30.55°, which correlates to the 78 plane of the anatase phase. The weeds, including Chenopodium album, Lathyrus aphaca, Angalis arvensis, and Melilotus indica, were sprayed with the nanoparticles while they were in the third or fourth leaf stage. There were seven distinct dosages used: doses (D0 (Check weeds), D1 (Recommended dose of traditional herbicide, D2 (Recommended dose of Nano-herbicide (NPs-H)), D3 (NPs-H with 05-fold lower dose), D4 ((NPs-H) with 10-fold lower dose), D5 (NPs-H with 15-fold lower dose), and D6 (NPs-H with 20-fold lower dose)). The chitosan-based nanoparticles of MCPA at the prescribed dosage of conventional herbicide resulted in complete death and visual damage, with a 100% fatality rate. The dosage that was 5-fold lower exhibited the lowest levels of plant height (3.95 cm), chlorophyll content (5.63%), dry biomass (0.10 g), and fresh biomass (0.33 g) in the broad-leaved weed of wheat. The herbicide nanoparticles, when used at a dosage 10-fold lower than that of conventional herbicides, had a comparable impact on the prescribed dosage. Nano-herbicides have the potential to improve the efficiency of standard herbicides by increasing stability and lowering toxicity.

Keywords: mortality, visual injury, chlorophyl contents, chitosan-based nanoparticles

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Authors: Raquel Galante, Marina Braga, Daniela Ghisleni, Terezinha J. A. Pinto, Rogério Colaço, Ana Paula Serro

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The sensitive nature of soft biomaterials, such as hydrogels, renders their sterilization a particularly challenging task for the biomedical industry. Widely used contact lenses are now studied as promising platforms for topical corneal drug delivery. However, to the best of the authors knowledge, the influence of sterilization methods on these systems has yet to be evaluated. The main goal of this study was to understand how different pairs drug-hydrogel would interact under an ozone-based sterilization method in comparison with two conventional processes (steam heat and gamma irradiation). For that, Si-Hy containing hydroxylethyl methacrylate (HEMA) and [tris(trimethylsiloxy)silyl]propyl methacrylate (TRIS) was produced and soaked in different drug solutions, commonly used for the treatment of ocular diseases (levofloxacin, chlorhexidine, diclofenac and timolol maleate). The drug release profiles and main material properties were evaluated before and after the sterilization. Namely, swelling capacity was determined by water uptake studies, transparency was accessed by UV-Vis spectroscopy, surface topography/morphology by scanning electron microscopy (SEM) and mechanical properties by performing tensile tests. The drug released was quantified by high performance liquid chromatography (HPLC). The effectiveness of the sterilization procedures was assured by performing sterility tests. Ozone gas method led to a significant reduction of drug released and to the formation of degradation products specially for diclofenac and levofloxacin. Gamma irradiation led to darkening of the loaded Si-Hys and to the complete degradation of levofloxacin. Steam heat led to smoother surfaces and to a decrease of the amount of drug released, however, with no formation of degradation products. This difference in the total drug released could be the related to drug/polymer interactions promoted by the sterilization conditions in presence of the drug. Our findings offer important insights that, in turn, could be a useful contribution to the safe development of actual products.

Keywords: drug delivery, silicone hydrogels, sterilization, gamma irradiation, steam heat, ozone gas

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Authors: H. Ferfera-Harrar, T. Benhalima, D. Lerari

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Contamination of water, due to the discharge of untreated industrial wastewaters into the ecosystem, has become a serious problem for many countries. In this study, bioadsorbents based on chitosan-g-poly(acrylamide) and montmorillonite (MMt) clay (CTS-g-PAAm/MMt) hydrogel nanocomposites were prepared via free‐radical grafting copolymerization and crosslinking of acrylamide monomer (AAm) onto natural polysaccharide chitosan (CTS) as backbone, in presence of various contents of MMt clay as nanofiller. Then, they were hydrolyzed to obtain highly functionalized pH‐sensitive nanomaterials with uppermost swelling properties. Their structure characterization was conducted by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) analyses. The adsorption performances of the developed nanohybrids were examined for removal of methylene blue (MB) cationic dye from aqueous solutions. The factors affecting the removal of MB, such as clay content, pH medium, adsorbent dose, initial dye concentration and temperature were explored. The adsorption process was found to be highly pH dependent. From adsorption kinetic results, the prepared adsorbents showed remarkable adsorption capacity and fast adsorption rate, mainly more than 88% of MB removal efficiency was reached after 50 min in 200 mg L^-1 of dye solution. In addition, the incorporating of various content of clay has enhanced adsorption capacity of CTS-g-PAAm matrix from 1685 to a highest value of 1749 mg g^-1 for the optimized nanocomposite containing 2 wt.% of MMt. The experimental kinetic data were well described by the pseudo-second-order model, while the equilibrium data were represented perfectly by Langmuir isotherm model. The maximum Langmuir equilibrium adsorption capacity (q_m) was found to increase from 2173 mg g⁻¹ until 2221 mg g⁻¹ by adding 2 wt.% of clay nanofiller. Thermodynamic parameters revealed the spontaneous and endothermic nature of the process. In addition, the reusability study revealed that these bioadsorbents could be well regenerated with desorption efficiency overhead 87% and without any obvious decrease of removal efficiency as compared to starting ones even after four consecutive adsorption/desorption cycles, which exceeded 64%. These results suggest that the optimized nanocomposites are promising as low cost bioadsorbents.

Keywords: chitosan, clay, dye adsorption, hydrogels nanocomposites

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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: 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: Hanaa A. Al-Gaoudi, Hassan Ebeid

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The research investigates the materials and processes used in the manufacturing of an Egyptian polychrome cartonnage mummy mask with the aim of dating this object and establishing trade patterns of certain materials that were used and available at the time of ancient Egypt. This anonymous-source object was held in the basement storage of the Egyptian Museum in Cairo (EMC) and has never been on display. Furthermore, there is no information available regarding its owner, provenance, date, and even the time of its possession by the museum. Moreover, the object is in a very poor condition where almost two-thirds of the mask was bent and has never received any previous conservation treatment. This research has utilized well-established multi-analytical methods to identify the considerable diversity of materials that have been used in the manufacturing of this object. These methods include Computed Tomography Scan (CT scan) to acquire detailed pictures of the inside physical structure and condition of the bended layers. Dino-Lite portable digital microscope, scanning electron microscopy with energy dispersive X-ray spectrometer (SEM-EDX), and the non-invasive imaging technique of multispectral imaging (MSI) to obtain information about the physical characteristics and condition of the painted layers and to examine the microstructure of the materials. Portable XRF Spectrometer (PXRF) and X-Ray powder diffraction (XRD) to identify mineral phases and the bulk element composition in the gilded layer, ground, and pigments; Fourier-transform infrared (FTIR) to identify organic compounds and their molecular characterization; accelerator mass spectrometry (AMS 14C) to date the object. Preliminary results suggest that there are no human remains inside the object, and the textile support is linen fibres with tabby weave 1/1 and these fibres are in a very bad condition. Several pigments have been identified, such as Egyptian blue, Magnetite, Egyptian green frit, Hematite, Calcite, and Cinnabar; moreover, the gilded layers are pure gold and the binding media in the pigments is Arabic gum and animal glue in the textile support layer.

Keywords: analytical methods, Egyptian museum, mummy mask, pigments, textile

Procedia PDF Downloads 124