Search results for: Scanning Electron Microscopy-Energy Dispersive Spectroscopy

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

Abstract:

In this work, the effect of particle size on the structural and magnetic properties of CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles synthesized by starch-assisted sol-gel auto combustion method was investigated. The different sized CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles were achieved after annealing at different temperature 500, 700 and 900 oC. The structural phases, crystallite size and lattice parameter of synthesized ferrite nanoparticles were estimated from X-ray diffraction studies. The field emission scanning electron microscopy study demonstrated increase in particle size with increase of annealing temperature. Raman spectroscopy study indicated the change in octahedral and tetrahedral site related Raman modes in Gd3+ ions doped cobalt ferrite nanoparticles. An infrared spectroscopy study showed the presence of two absorption bands in the frequency range around 580 cm-1 (ν1) and around 340 cm-1 (ν2); which indicated the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Vibrating Sample magnetometer study showed that the saturation magnetization and coercivity changes with particle size of CoFe2-xGdxO4 (x =0.1) spinel ferrite.

Keywords: magnetic properties, spinel ferrite, nanoparticles, sol-gel synthesis

Procedia PDF Downloads 492

Authors: Afifa Hafidh, Fathi Touati, Ahmed Hichem Hamzaoui, Sayda Somrani

Abstract:

The objective of the present study has been to synthesize and to characterize silica hybrid materials using sol-gel technic and to investigate their properties. Silica materials were successfully fabricated using various bi-functional 1,3,4-thiadiazoles and tetraethoxysilane (TEOS) as co-precursors via a facile one-pot sol-gel pathway. TEOS was introduced at room temperature with 1,3,4-thiadiazole 2,5-difunctiunal adducts, in ethanol as solvent and using HCl acid as catalyst. The sol-gel process lead to the formation of monolithic, coloured and transparent gels. TEOS was used as a principal network forming agent. The incorporation of 1,3,4-thiadiazole molecules was realized by attachment of these later onto a silica matrix. This allowed covalent linkage between organic and inorganic phases and lead to the formation of Si-N and Si-S bonds. The prepared hybrid materials were characterized by Fourier transform infrared, NMR ²⁹Si and ¹³C, scanning electron microscopy and nitrogen absorption-desorption measurements. The optic and magnetic properties of hybrids are studied respectively by ultra violet-visible spectroscopy and electron paramagnetic resonance. It was shown in this work, that heterocyclic moieties were successfully attached in the hybrid skeleton. The formation of the Si-network composed of cyclic units (Q3 structures) connected by oxygen bridges (Q4 structures) was proved by ²⁹Si NMR spectroscopy. The Brunauer-Elmet-Teller nitrogen adsorption-desorption method shows that all the prepared xerogels have isotherms type IV and are mesoporous solids. The specific surface area and pore volume of these materials are important. The obtained results show that all materials are paramagnetic semiconductors. The data obtained by Nuclear magnetic resonance ²⁹Si and Fourier transform infrared spectroscopy, show that Si-OH and Si-NH groups existing in silica hybrids can participate in adsorption interactions. The obtained materials containing reactive centers could exhibit adsorption properties of metal ions due to the presence of OH and NH functionality in the mesoporous frame work. Our design of a simple method to prepare hybrid materials may give interest of the development of mesoporous hybrid systems and their use within the domain of environment in the future.

Keywords: hybrid materials, sol-gel process, 1, 3, 4-thiadaizole, TEOS

Procedia PDF Downloads 183

Authors: Abhishek Soti, Aditya Sharma, Akhilendra Bhushan Gupta

Abstract:

Fouled reverse osmosis membranes are primarily characterized by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectrometer (EDS) for a detailed investigation of foulants; however, this has severe limitations on several accounts. Apart from inaccuracy in spectral properties and inevitable interferences and interactions between sample and instrument, misidentification of elements due to overlapping peaks is a significant drawback of EDS. This paper discusses this limitation by analyzing fouled polyamide RO membranes derived from community RO plants of Rajasthan treating brackish water via a combination of results obtained from EDS and Raman spectroscopy and cross corroborating with ICP-MS analysis of water samples prepared by dissolving the deposited salts. The anomalous behavior of different morphic forms of CaCO₃ in aqueous suspensions tends to introduce false reporting of the presence of certain heavy metals and rare earth metals in the scales of the fouled RO membranes used for treating brackish groundwater when analyzed using the commonly adopted techniques like SEM-EDS or Raman spectrometry. Peaks of CaCO₃ reflected in EDS spectra of the membrane were found to be misinterpreted as Scandium due to the automatic assignment of elements by the software. Similarly, the morphic forms merged with the dominant peak of CaCO₃ might be reflected as a single peak of Molybdenum in the Raman spectrum. A subsequent ICP-MS analysis of the deposited salts showed that both Sc and Mo were below detectable levels. It is always essential to cross-confirm the results through a destructive analysis method to avoid such interferences. It is further recommended to study different morphic forms of CaCO₃ scales, as they exhibit anomalous properties like reverse solubility with temperature and hence altered precipitation tendencies, for an accurate description of the composition of scales, which is vital for the smooth functioning of RO systems.

Keywords: reverse osmosis, foulant analysis, groundwater, EDS, artifacts

Procedia PDF Downloads 106

Authors: Vishal Kumar Gupta

Abstract:

Purpose: This study has been undertaken to develop novel pH sensitive interpenetrating network hydrogel beads. Methods: The pH sensitive PAAM-g-Guar gum copolymer was synthesized by free radical polymerization followed by alkaline hydrolysis. Beads of guar gum-grafted-polyacrylamide and sodium Carboxy methyl cellulose (Na CMC) loaded with Pantoprazole sodium were prepared and evaluated for pH sensitivity, swelling properties, drug entrapment efficiency and in vitro drug release characteristics. Seven formulations were prepared for the drug with varying polymer and cross linker concentrations. Results: The grafting and alkaline hydrolysis reactions were confirmed by FT-IR spectroscopy. Differential scanning calorimetry was carried out to know the compatibility of encapsulated drug with the polymers. Scanning electron microscopic study revealed that the IPN beads were spherical. The entrapment efficiency was found to be in the range of 85-92%. Particle size analysis was carried out by optical microscopy. As the pH of the medium was changed from 1.2 to 7.4, a considerable increase in swelling was observed for all beads. Increase in the copolymer concentration showed sustained the drug release up to 12 hrs. Drug release from the beads followed super case II transport mechanism. Conclusion: It was concluded that guar gum-acrylamide beads, cross-linked with aluminum chloride offer an opportunity for controlled drug release of pantoprazole sodium.

Keywords: IPN, hydrogels, DSC, SEM

Procedia PDF Downloads 269

Authors: Seyfullah Madakbaş, Ferhat Şen, Memet Vezir Kahraman

Abstract:

The aim of this study was to improve thermal stability, mechanical and surface properties of thermoplastic polyurethane (TPU) with the addition of BaTiO3. The TPU/ BaTiO3 composites having various ratios of TPU and BaTiO3 were prepared. The chemical structure of the prepared composites was investigated by FT-IR. FT-IR spectra of TPU/ barium titanate composites show that they successfully were prepared. Thermal stability of the samples was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The prepared composites showed high thermal stability, and the char yield increased as barium titanate content increased. The glass transition temperatures of the composites rise with the addition of barium titanate. Mechanical properties of the samples were characterized with stress-strain test. The mechanical properties of the TPU were increased with the contribution of the contribution of the barium titanate it increased. Hydrophobicity of the samples was determined by the contact angle measurements. The contact angles have the tendency to increase the hydrophobic behavior on the surface, when barium titanate was added into TPU. Moreover, the surface morphology of the samples was investigated by a scanning electron microscopy (SEM). SEM-EDS mapping images showed that barium titanate particles were dispersed homogeneously. Finally, the obtained results prove that the prepared composites have good thermal, mechanical and surface properties and that they can be used in many applications such as the electronic devices, materials engineering and other emergent.

Keywords: barium titanate, composites, thermoplastic polyurethane, scanning electron microscopy

Procedia PDF Downloads 329

Authors: Indah Kurniawaty, Yoki Yulizar, Haryo Satriya Oktaviano, Adam Kusuma Rianto

Abstract:

Magnesium oxide nanoparticles (MgO NP) were successfully synthesized in this study using a one-pot green synthesis mediated by Calliandra Calothyrsus leaf extract (CLE). CLE was prepared by maceration of the leaf using methanol with a ratio of 1:5 for 7 days. Secondary metabolites in CLE, such as alkaloids and flavonoids, served as a weak base provider and capping agent in the formation of MgO NP. CLE Fourier Transform Infra-Red (FTIR) spectra peak at 3255, 1600, 1384, 1205, 1041, and 667 cm-1 showing the presence of vibrations O-H stretching, N-H bending, C-C stretching, C-N stretching and N-H wagging. During the experiment, different CLE volumes and calcined temperatures were used, resulting in a variety of structures. Energy Dispersive X-ray Spectrometer (EDS) and FTIR were used to characterize metal oxide particles. MgO diffraction pattern at 2θ of 36.9°; 42.9°; 62.2°; 74.6°; and 78.5° which can be assigned to crystal planes (111), (200), (220), (311), and (222), respectively. Scanning Electron Microscopy (SEM) was used to characterize the surface morphology. The morphology ranged from sphere to flower-like resulting in crystallite sizes of 28, 23, 12, and 9 nm.

Keywords: MgO, nanoparticle, calliandra calothyrsus, green-synthesis

Procedia PDF Downloads 81

Authors: Supriya Mahida, Sangita, Yogesh U. Shah, Shanta Kumar

Abstract:

The global production of thermocol increasing day by day, due to vast applications of the use of thermocole in many sectors. Thermocol being non-biodegradable and more toxic than plastic leads towards a number of problems like its management into value-added products, environmental damage and landfill problems due to weight to volume ratio. Utilization of waste thermocol for modification of bitumen binders resulted in waste thermocol modified bitumen (WTMB) used in road construction and maintenance technology. Modification of bituminous mixes through incorporating thermocol into bituminous mixes through a dry process is one of the new options besides recycling process which consumes lots of waste thermocol. This process leads towards waste management and remedies against thermocol waste disposal. The present challenge is to dispose the thermocol waste under different forms in road infrastructure, either through the dry process or wet process to be developed in future. This paper focuses on the use of thermocol wastes which is mixed with VG 10 bitumen in proportions of 0.5%, 1%, 1.5%, and 2% by weight of bitumen. The physical properties of neat bitumen are evaluated and compared with modified VG 10 bitumen having thermocol. Empirical characterization like penetration, softening, and viscosity of bitumen has been carried out. Thermocol and waste thermocol modified bitumen (WTMB) were further analyzed by Fourier Transform Infrared Spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), and Dynamic Shear Rheometer (DSR).

Keywords: DSR, FESEM, FT-IR, thermocol wastes

Procedia PDF Downloads 167

Authors: S. Alrekabi, A. Cundy, A. Lampropoulos, I. Savina

Abstract:

Due to their remarkable mechanical properties, multi-wall carbon nanotubes (MWCNTs) are considered by many researchers to be a highly promising filler and reinforcement agent for enhanced performance cementitious materials. Currently, however, achieving an effective dispersion of MWCNTs remains a major challenge in developing high performance nano-cementitious composites, since carbon nanotubes tend to form large agglomerates and bundles as a consequence of Van der Waals forces. In this study, effective dispersion of low concentrations of MWCNTs at 0.01%, 0.025%, and 0.05% by weight of cement in the composite was achieved by applying different sonication conditions in combination with the use of polycarboxylate ether as a surfactant. UV-Visible spectroscopy and Transmission electron microscopy (TEM) were used to assess the dispersion of MWCNTs in water, while the dispersion states of MWCNTs within the cement composites and their surface interactions were examined by scanning electron microscopy (SEM). A high sonication intensity applied over a short time period significantly enhanced the dispersion of MWCNTs at initial mixing stages, and 0.025% of MWCNTs wt. of cement, caused 86% and 27% improvement in tensile strength and compressive strength respectively, compared with a plain cement mortar.

Keywords: dispersion, mechanical performance, multi wall carbon nanotubes, sonication conditions

Procedia PDF Downloads 321

Authors: El-Said I. El-Shafey, Syeda Naheed F. Ali, Saleh S. Al-Busafi, Haider A. J. Al-Lawati

Abstract:

Date palm leaflets were utilized as a precursor for activated carbon (AC) preparation using KOH activation. AC produced was oxidized using nitric acid producing oxidized activated carbon (OAC). OAC that possesses acidic surface was surface functionalized to produce basic activated carbons using linear diamine compounds (ethylene diamine and propylene diamine). OAC was also functionalized to produce hydrophobic activated carbons using ethylamine (EA) and aniline (AN). Dehydrated carbon was also prepared from date palm leaflets using sulfuric acid dehydration/ oxidation and was surface functionalized in the same way as AC. Nitric acid oxidation was not necessary for DC as it is acidic carbon. The surface area of AC is high (823 m2/g) with microporosity domination, however, after oxidation and surface functionalization, both the surface area and surface microporosity decrease tremendously. DC surface area was low (15 m2/g) with mesoporosity domination. Surface functionalization has decreased the surface area of activated carbons. FTIR spectra show that -COOH group on DC and OAC almost disappeared after surface functionalization. The surface chemistry of all carbons produced was tested for pHzpc, basic sites, boehm titration, thermogravimetric analysis and zeta potential measurement. Scanning electron microscopy and energy dispersive spectroscopy in addition to CHN elemental analysis were also carried out. DC and OAC possess low pHzpc and high surface functionality, however, basic and hydrophobic carbons possess high pHzpc and low surface functionality. The different behavior of carbons is related to their different surface chemistry. Methylene blue adsorption was found to be faster on hydrophobic carbons based on AC and DC. The Larger adsorption capacity of methylene blue was found for hydrophobic carbons. Dominating adsorption forces of methylene blue varies from carbon to another depending on its surface nature. Sorption forces include hydrophobic forces, H-bonding, electrostatic interactions and van der Waals forces.

Keywords: carbon, acidic, basic, hydrophobic

Procedia PDF Downloads 286

Authors: S. Mohajeri

Abstract:

Electrocodeposition of Ni-TiO2 nanocomposite single layers and Ni-TiO2/TiO2 multilayers from Watts bath containing TiO2 sol was carried out on copper substrate. Pulse plating and pulse reverse plating techniques were applied to facilitate higher incorporations of TiO2 nanoparticles in Ni-TiO2 nanocomposite single layers, and the results revealed that by prolongation of the current-off durations and the anodic cycles, deposits containing 11.58 wt.% and 13.16 wt.% TiO2 were produced, respectively. Multilayer coatings which consisted of Ni-TiO2 and TiO2-rich layers were deposited by pulse potential deposition through limiting the nickel deposition by diffusion control mechanism. The TiO2-rich layers thickness and accordingly, the content of TiO2 reinforcement reached 104 nm and 18.47 wt.%, respectively in the optimum condition. The phase structure and surface morphology of the nanocomposite coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cross sectional morphology and line scans of the layers were studied by field emission scanning electron microscopy (FESEM). It was confirmed that the preferred orientations and the crystallite sizes of nickel matrix were influenced by the deposition technique parameters, and higher contents of codeposited TiO2 nanoparticles refined the microstructure. The corrosion behavior of the coatings in 1M NaCl and 0.5M H2SO4 electrolytes were compared by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. Increase of corrosion resistance and the passivation tendency were favored by TiO2 incorporation, while the degree of passivation declined as embedded particles disturbed the continuity of passive layer. The role of TiO2 incorporation on the improvement of mechanical properties including hardness, elasticity, scratch resistance and friction coefficient was investigated by the means of atomic force microscopy (AFM). Hydrophilicity and wettability of the composite coatings were investigated under UV illumination, and the water contact angle of the multilayer was reduced to 7.23° after 1 hour of UV irradiation.

Keywords: electrodeposition, hydrophilicity, multilayer, pulse-plating

Procedia PDF Downloads 252

Authors: Ravi V. Joat, Pravin S. Bodke, Shradha S. Binani, S. S. Wasnik

Abstract:

A phase diagram of the Ag2SO4 - CaSO4 (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag2SO4 + CaSO4) is observed at 10 mole% CaSO4 and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca 2+ in Ag2SO4 is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO4 content. Amongst other binary compositions, the 80AgSO4-20CaSO4 gave improved sinterability/packing density.

Keywords: phase diagram, Ag2SO4-CaSO4 binaries system, conductivity, XRD, DTA

Procedia PDF Downloads 627

Authors: Mehdi Rahimi-Nasrabadi, Seied Mahdi Pourmortazavi

Abstract:

Taguchi robust design as a statistical method was applied for optimization of the process parameters in order to tunable, simple and fast synthesis of europium (III) tungstate nanoparticles. Europium (III) tungstate nanoparticles were synthesized by a chemical precipitation reaction involving direct addition of europium ion aqueous solution to the tungstate reagent solved in aqueous media. Effects of some synthesis procedure variables i.e., europium and tungstate concentrations, flow rate of cation reagent addition, and temperature of reaction reactor on the particle size of europium (III) tungstate nanoparticles were studied experimentally in order to tune particle size of europium (III) tungstate. Analysis of variance shows the importance of controlling tungstate concentration, cation feeding flow rate and temperature for preparation of europium (III) tungstate nanoparticles by the proposed chemical precipitation reaction. Finally, europium (III) tungstate nanoparticles were synthesized at the optimum conditions of the proposed method and the morphology and chemical composition of the prepared nano-material were characterized by means of X-Ray diffraction, scanning electron microscopy, transmission electron microscopy, FT-IR spectroscopy, and fluorescence.

Keywords: europium (III) tungstate, nano-material, particle size control, procedure optimization

Procedia PDF Downloads 395

Authors: Mookyada Mankrut, Manit Nithitanakul

Abstract:

An increase in the amount of atmospheric carbon dioxide (CO2) resulting from anthropogenic CO2 emission has been a concerned problem so far. Adsorption using porous materials is feasible way to reduce the content of CO2 emission into the atmosphere due to several advantages: low energy consumption in regeneration process, low-cost raw materials and, high CO2 adsorption capacity. In this work, the porous poly(divinylbenzene) (poly(DVB)) support was synthesized under high internal phase emulsion (HIPE) polymerization then modified with polyethyleneimine (PEI) by using solution plasma process. These porous polymers were then used as adsorbents for CO2 adsorption study. All samples were characterized by some techniques: Fourier transform infrared spectroscopy (FT-IR), scanning electron spectroscopy (SEM), water contact angle measurement and, surface area analyzer. The results of FT-IR and a decrease in contact angle, pore volume and, surface area of PEI-loaded materials demonstrated that surface of poly(DVB) support was modified. In other words, amine groups were introduced to poly(DVB) surface. In addition, not only the outer surface of poly(DVB) adsorbent was modified, but also the inner structure as shown by FT-IR study. As a result, PEI-loaded materials exhibited higher adsorption capacity, comparing with those of the unmodified poly(DVB) support.

Keywords: polyHIPEs, CO2 adsorption, solution plasma process, high internal phase emulsion

Procedia PDF Downloads 273

Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

Abstract:

Herein, we reported the influence of La³⁺ substitution on structural, magnetic and dielectric properties of CoFe₂O₄ nanoparticles synthesized by starch-assisted sol-gel combustion method. X-ray diffraction pattern confirmed the formation of cubic spinel structure of La³⁺ ions doped CoFe₂O₄ nanoparticles. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of La³⁺ substituted CoFe₂O₄ nanoparticles. The field emission scanning electron microscopy study revealed that La³⁺ substituted CoFe2O4 nanoparticles were in the range of 10-40 nm. The magnetic properties of La³⁺ substituted CoFe₂O₄ nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with La³⁺ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied with change of concentration of La³⁺ ions in CoFe₂O₄ nanoparticles. The variation in optical properties was studied via UV-Vis absorption spectroscopy. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: starch, sol-gel combustion method, nanoparticles, magnetic properties, dielectric properties

Procedia PDF Downloads 315

Authors: L. Pu, C. Unluer

Abstract:

MgO cements have the potential to sequester CO2 in construction products, and can be partial or complete replacement of PC in concrete. Construction block is a promising application for reactive MgO cements. Main advantages of blocks are: (i) suitability for sequestering CO2 due to their initially porous structure; (ii) lack of need for in-situ treatment as carbonation can take place during fabrication; and (iii) high potential for commercialization. Both strength gain and carbon sequestration of MgO cements depend on carbonation process. Fly ash and ground granulated blast-furnace slag (GGBS) are pozzolanic material and are proved to improve many of the performance characteristics of the concrete, such as strength, workability, permeability, durability and corrosion resistance. A very limited amount of work has been reported on the production of MgO blocks on a large scale so far. A much more extensive study, wherein blocks with different mix design is needed to verify the feasibility of commercial production. The changes in the performance of the samples were evaluated by compressive strength testing. The properties of the carbonation products were identified by X-ray diffraction (XRD) and scanning electron microscopy (SEM)/ field emission scanning electron microscopy (FESEM), and the degree of carbonation was obtained by thermogravimetric analysis (TGA), XRD and energy dispersive X-ray (EDX). The results of this study enabled the understanding the relationship between lab-scale samples and scale-up blocks based on their mechanical performance and microstructure. Results indicate that for both scaled-up and lab-scale samples, MgO samples always had the highest strength results, followed by MgO-fly ash samples and MgO-GGBS had relatively lowest strength. The lower strength of MgO with fly ash/GGBS samples at early stage is related to the relatively slow hydration process of pozzolanic materials. Lab-scale cubic samples were observed to have higher strength results than scaled-up samples. The large size of the scaled-up samples made it more difficult to let CO2 to reach inner part of the samples and less carbonation products formed. XRD, TGA and FESEM/EDX results indicate the existence of brucite and HMCs in MgO samples, M-S-H, hydrotalcite in the MgO-fly ash samples and C-S-H, hydrotalctie in the MgO-GGBS samples. Formation of hydration products (M-S-H, C-S-H, hydrotalcite) and carbonation products (hydromagnecite, dypingite) increased with curing duration, which is the reason of increasing strength. This study verifies the advantage of large-scale MgO blocks over common PC blocks and the feasibility of commercial production of MgO blocks.

Keywords: reactive MgO, fly ash, ground granulated blast-furnace slag, carbonation, CO₂

Procedia PDF Downloads 192

Authors: Ambrish Singh

Abstract:

The corrosion inhibition performance of pyran derivatives (AP) on mild steel in 15% HCl was investigated by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization, weight loss, contact angle, and scanning electron microscopy (SEM) measurements, DFT and molecular dynamic simulation. The adsorption of APs on the surface of mild steel obeyed Langmuir isotherm. The potentiodynamic polarization study confirmed that inhibitors are mixed type with cathodic predominance. Molecular dynamic simulation was applied to search for the most stable configuration and adsorption energies for the interaction of the inhibitors with Fe (110) surface. The theoretical data obtained are, in most cases, in agreement with experimental results.

Keywords: acidizing inhibitor, pyran derivatives, DFT, molecular simulation, mild steel, EIS

Procedia PDF Downloads 198

Authors: Soad Abubakr Abdelgalil, Gaber Attia Abo-Zaid, Mohamed Mohamed Yousri Kaddah

Abstract:

Background: The Environmental Protection Agency has listed eggshell waste as the 15th most significant food industry pollution hazard. The utilization of eggshell waste as a source of renewable energy has been a hot topic in recent years. Therefore, finding a sustainable solution for the recycling and valorization of eggshell waste by investigating its potential to produce acid phosphatase (ACP) and organic acids by the newly-discovered B. sonorensis was the target of the current investigation. Results: The most potent ACP-producing B. sonorensis strain ACP2 was identified as a local bacterial strain obtained from the effluent of paper and pulp industries on basis of molecular and morphological characterization. The use of consecutive statistical experimental approaches of Plackett-Burman Design (PBD), and Orthogonal Central Composite Design (OCCD), followed by pH-uncontrolled cultivation conditions in a 7 L bench-top bioreactor, revealed an innovative medium formulation that substantially improved ACP production, reaching 216 U L⁻¹ with ACP yield coefficient Yp/x of 18.2 and a specific growth rate (µ) of 0.1 h⁻¹. The metals Ag+, Sn+, and Cr+ were the most efficiently released from eggshells during the solubilization process by B. sonorensis. The uncontrolled pH culture condition is the most suited and favored setting for improving the ACP and organic acids production simultaneously. Quantitative and qualitative analyses of produced organic acids were carried out using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Lactic acid, citric acid, and hydroxybenzoic acid isomer were the most common organic acids produced throughout the cultivation process. The findings of thermogravimetric analysis (TGA), differential scan calorimeter (DSC), scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), Fourier-Transform Infrared Spectroscopy (FTIR), and X-Ray Diffraction (XRD) analysis emphasize the significant influence of organic acids and ACP activity on the solubilization of eggshells particles. Conclusions: This study emphasized robust microbial engineering approaches for the large-scale production of a newly discovered acid phosphatase accompanied by organic acids production from B. sonorensis. The biovalorization of the eggshell waste and the production of cost-effective ACP and organic acids were integrated into the current study, and this was done through the implementation of a unique and innovative medium formulation design for eggshell waste management, as well as scaling up ACP production on a bench-top scale.

Keywords: chicken eggshells waste, bioremediation, statistical experimental design, batch fermentation

Procedia PDF Downloads 376

Authors: José M. Liñeira Del Río, Ramón Rial, Khodor Nasser, María J.G. Guimarey

Abstract:

The need to develop new lubricants that offer better anti-friction and anti-wear performance in internal combustion vehicles is one of the great challenges of lubrication in the automotive field. The addition of nanoparticles has emerged as a possible solution and, combined with the lubricating power of ionic liquids, may become one of the alternatives to reduce friction losses and wear of the contact surfaces in the conditions to which tribo-pairs are subjected, especially in the contact of the piston rings and the cylinder liner surface. In this study, the improvement in SAE 10W-40 engine oil tribological performance after the addition of magnesium oxide (MgO) nanoadditives and two different phosphonium-based ionic liquids (ILs) was investigated. The nanoparticle characterization was performed by means of transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The tribological properties, friction coefficients and wear parameters of the formulated oil modified with 0.01 wt.% MgO and 1 wt.% ILs compared with the neat 10W-40 oil were performed and analyzed using a ball-on-three-pins tribometer and a 3D optical profilometer, respectively. Further analysis on the worn surface was carried out by Raman spectroscopy and SEM microscopy, illustrating the formation of the protective IL and MgO tribo-films as hybrid additives. In friction tests with sliding steel-steel tribo-pairs, IL3-based hybrid nanolubricant decreased the friction coefficient and wear volume by 7% and 59%, respectively, in comparison with the neat SAE 10W-40, while the one based on IL1 only achieved a reduction of these parameters by 6% and 39%, respectively. Thus, the tribological characterization also revealed that the MgO and IL3 addition has a positive synergy over the commercial lubricant, adequately meeting the requirements for their use in internal combustion engines. In summary, this study has shown that the addition of ionic liquids to MgO nanoparticles can improve the stability and lubrication behavior of MgO nanolubricant and encourages more investigations on using nanoparticle additives with green solvents such as ionic liquids to protect the environment as well as prolong the lifetime of machinery. The improvement in the lubricant properties was attributed to the following wear mechanisms: the formation of a protective tribo-film and the ability of nanoparticles to fill out valleys between asperities, thereby effectively smoothing out the shearing surfaces.

Keywords: lubricant, nanoparticles, phosphonium-based ionic liquids, tribology

Procedia PDF Downloads 82

Authors: Fuad Abdullah Alatawi

Abstract:

Microbial infections-based diseases are a significant public health issue around the world, mainly when antibiotic-resistant bacterium types evolve. In this research, we explored the anti-bacterial and anti-cancer potency of iron-oxide (Fe₂O₃) nanoparticles prepared from F. macrocarpa fruit extract. The chemical composition of F. macrocarpa fruit extract was used as a reducing and capping agent for nanoparticles’ synthesis was examined by GC-MS/MS analysis. Then, the prepared nanoparticles were confirmed by various biophysical techniques, including X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), UV-Vis Spectroscopy, and Transmission Electron Microscopy (TEM) and Energy Dispersive Spectroscopy (EDAX), and Dynamic Light Scattering (DLS). Also, the antioxidant capacity of fruit extract was determined through 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS), Fluorescence Recovery After Photobleaching (FRAP), Superoxide Dismutase (SOD) assays. Furthermore, the cytotoxicity activities of Fe₂O₃ NPs were determined using the (3-(4, 5-dimethylthiazolyl-2)-2, 5-diphenyltetrazolium bromide) (MTT) test on MCF-7 cells. In the antibacterial assay, lethal doses of the Fe₂O₃NPs effectively inhibited the growth of gram-negative and gram-positive bacteria. The surface damage, ROS production, and protein leakage are the antibacterial mechanisms of Fe₂O₃NPs. Concerning antioxidant activity, the fruit extracts of F. macrocarpa had strong antioxidant properties, which were confirmed by DPPH, ABTS, FRAP, and SOD assays. In addition, the F. microcarpa-derived iron oxide nanomaterials greatly reduced the cell viability of (MCF-7). The GC-MS/MS analysis revealed the presence of 25 main bioactive compounds in the F. microcarpa extract. Overall, the finding of this research revealed that F. microcarpa-derived Fe₂O₃ nanoparticles could be employed as an alternative therapeutic agent to cure microbial infection and breast cancer in humans.

Keywords: ficus microcarpa, iron oxide, antibacterial activity, cytotoxicity

Procedia PDF Downloads 123

Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

Abstract:

The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

Procedia PDF Downloads 143

Authors: G. Nyongombe, Guy L. Kabongo, B. M. Mothudi, M. S. Dhlamini

Abstract:

A series of Transition Metals Oxides (TMOs) doped graphene were synthesized and successfully used as supercapacitor electrode materials. The as-synthesized materials exhibited exceptional electrochemical properties owing to the combined properties of its constituents; high surface area and good conductivity were achieved. Several analytical characterization techniques were employed to investigate the morphology, crystal structure atomic arrangement and elemental chemical state in the materials for which scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were conducted, respectively. Moreover, the electrochemical properties of the as-synthesized materials were examined by performing cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) measurements. Furthermore, the effect of doping concentration on the interlayer distance of the graphene materials and the charge transfer resistance are investigated and correlated to the exceptional current density which was multiplied by a factor of ~80 after TMOs doping in graphene. Finally, the resulting high capacitance obtained confirms the contribution of grapheme exceptional electronic conductivity and large surface area on the electrode materials. Such good-performing electrode materials are highly promising for supercapacitors and other energy storage devices.

Keywords: energy density, graphene, supercapacitors, TMOs

Procedia PDF Downloads 258

Authors: Adinarayana Gorajana, Venkata Srikanth Meka, Sanjay Garg, Lim Sue May

Abstract:

This study was designed to evaluate and enhance the solubility of poorly soluble drug, docetaxel through solid dispersion (SD) technique prepared using freeze drying method. Docetaxel solid dispersions were formulated with Soluplus in different weight ratios. Freeze drying method was used to prepare the solid dispersions. Solubility of the solid dispersions were evaluated respectively and the optimized of drug-solubilizers ratio systems were characterized with different analytical methods like Differential scanning calorimeter (DSC), Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) to confirm the formation of complexes between drug and solubilizers. The solubility data revealed an overall improvement in solubility for all SD formulations. The ternary combination 1:5:2 gave the highest increase in solubility that is approximately 3 folds from the pure drug, suggesting the optimum drug-solubilizers ratio system. This data corresponds with the DSC and SEM analyses, which demonstrates presence of drug in amorphous state and the dispersion in the solubilizers in molecular level. The solubility of the poorly soluble drug, docetaxel was enhanced through preparation of solid dispersion formulations employing freeze drying method. Solid dispersion with multiple carrier system shows better solubility compared to single carrier system.

Keywords: docetaxel, freeze drying, soluplus, solid dispersion technique

Procedia PDF Downloads 504

Authors: Pachari Chuenta, Suwat Nanan

Abstract:

ZnO nanostructures have been synthesized successfully in high yield via catalyst-free chemical precipitation technique by varying zinc source (either zinc nitrate or zinc acetate) and oxygen source (either oxalic acid or urea) without using any surfactant, organic solvent or capping agent. The ZnO nanostructures were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), UV-vis diffuse reflection spectroscopy (UV-vis DRS), and photoluminescence spectroscopy (PL). The FTIR peak in the range of 450-470 cm-1 corresponded to Zn-O stretching in ZnO structure. The synthesized ZnO samples showed well crystalized hexagonal wurtzite structure. SEM micrographs displayed spherical droplet of about 50-100 nm. The band gap of prepared ZnO was found to be 3.4-3.5 eV. The presence of PL peak at 468 nm was attributed to surface defect state. The photocatalytic activity of ZnO was studied by monitoring the photodegradation of reactive red (RR141) azo dye under ultraviolet (UV) light irradiation. Blank experiment was also separately carried out by irradiating the aqueous solution of the dye in absence of the photocatalyst. The initial concentration of the dye was fixed at 10 mgL-1. About 50 mg of ZnO photocatalyst was dispersed in 200 mL dye solution. The sample was collected at a regular time interval during the irradiation and then was analyzed after centrifugation. The concentration of the dye was determined by monitoring the absorbance at its maximum wavelength (λₘₐₓ) of 544 nm using UV-vis spectroscopic analysis technique. The sources of Zn and O played an important role on photocatalytic performance of the ZnO photocatalyst. ZnO nanoparticles which prepared by zinc acetate and oxalic acid at molar ratio of 1:1 showed high photocatalytic performance of about 97% toward photodegradation of reactive red azo dye (RR141) under UV light irradiation for only 60 min. This work demonstrates the promising potential of ZnO nanomaterials as photocatalysts for environmental remediation.

Keywords: azo dye, chemical precipitation, photocatalytic, ZnO

Procedia PDF Downloads 144

Authors: Asad Hanif, Pavithra Parthasarathy, Zongjin Li

Abstract:

Thermal insulating composites help to reduce the total power consumption in a building by creating a barrier between external and internal environment. Such composites can be used in the roofing tiles or wall panels for exterior surfaces. This study purposes to develop lightweight cement-based composites for thermal insulating applications. Waste materials like silica fume (an industrial by-product) and fly ash cenosphere (FAC) (hollow micro-spherical shells obtained as a waste residue from coal fired power plants) were used as partial replacement of cement and lightweight filler, respectively. Moreover, aerogel, a nano-porous material made of silica, was also used in different dosages for improved thermal insulating behavior, while poly vinyl alcohol (PVA) fibers were added for enhanced toughness. The raw materials including binders and fillers were characterized by X-Ray Diffraction (XRD), X-Ray Fluorescence spectroscopy (XRF), and Brunauer–Emmett–Teller (BET) analysis techniques in which various physical and chemical properties of the raw materials were evaluated like specific surface area, chemical composition (oxide form), and pore size distribution (if any). Ultra-lightweight cementitious composites were developed by varying the amounts of FAC and aerogel with 28-day unit weight ranging from 1551.28 kg/m³ to 1027.85 kg/m³. Excellent mechanical and thermal insulating properties of the resulting composites were obtained ranging from 53.62 MPa to 8.66 MPa compressive strength, 9.77 MPa to 3.98 MPa flexural strength, and 0.3025 W/m-K to 0.2009 W/m-K as thermal conductivity coefficient (QTM-500). The composites were also tested for peak temperature difference between outer and inner surfaces when subjected to heating (in a specially designed experimental set-up) by a 275W infrared lamp. The temperature difference up to 16.78 ^oC was achieved, which indicated outstanding properties of the developed composites to act as a thermal barrier for building envelopes. Microstructural studies were carried out by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) for characterizing the inner structure of the composite specimen. Also, the hydration products were quantified using the surface area mapping and line scale technique in EDS. The microstructural analyses indicated excellent bonding of FAC and aerogel in the cementitious system. Also, selective reactivity of FAC was ascertained from the SEM imagery where the partially consumed FAC shells were observed. All in all, the lightweight fillers, FAC, and aerogel helped to produce the lightweight composites due to their physical characteristics, while exceptional mechanical properties, owing to FAC partial reactivity, were achieved.

Keywords: aerogel, cement-based, composite, fly ash cenosphere, lightweight, sustainable development, thermal conductivity

Procedia PDF Downloads 225

Authors: C.W. Kan

Abstract:

This paper investigates the use of atmospheric pressure plasma for improving the surface hydrophobicity of polyurethane synthetic leather with tetramethylsilane (TMS). The atmospheric pressure plasma treatment with TMS is a single-step process to enhance the hydrophobicity of polyurethane synthetic leather. The hydrophobicity of the treated surface was examined by contact angle measurement. The physical and chemical surface changes were evaluated by scanning electron microscopy (SEM) and infrared spectroscopy (FTIR). The purpose of this paper is to provide learning materials for understanding how to use atmospheric pressure plasma in the textile finishing process to transform a hydrophilic surface to hydrophobic.

Keywords: Learning materials, atmospheric pressure plasma treatment, hydrophobic, hydrophilic, surface

Procedia PDF Downloads 355

Authors: Erfan Rahimi, Hadi Bahari Far, Mojgan Shikhpour

Abstract:

Background: Urinary tract infection is one of the most common nosocomial infections, especially among women. E. coli is one of the main causes of urinary tract infections and one of the most common antibiotics to fight this bacterium is ampicillin. As conventional antibiotics led to bacterial antibiotic resistance, modification of the pure drugs can address this issue. The aim of this study was to prepare nanofluids containing carbon nanotubes conjugated with ampicillin to improve drug performance and reduce antibiotic resistance. Methods: Multi-walled carbon nanotubes (MWCNTs) were activated with thionyl chloride by reflux system and nanofluids containing antibiotics were prepared by ultrasonic method. The properties of the prepared nano-drug were investigated by general element analysis, infrared spectroscopy, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy. After the treatment of the desired strain with nanofluid, microbial studies were performed to evaluate the antibacterial effects and molecular studies were carried out to measure the expression of the resistance gene AcrAB. Result: We have shown that the antimicrobial effect of ampicillin-functionalized MWCNTs at low concentrations performed better than that of the conventional drug in both resistant and ATCC strains. Also, a decrease in antibiotic resistance of bacteria treated with ampicillin-functionalized MWCNTs compared to the pure drug was observed. Also, ampicillin-functionalized MWCNTs downregulated the expression of AcrAB in treated bacteria. Conclusion: Because carbon nanotubes are capable of destroying the bacterial wall, which provides antibiotic resistance features in bacteria, their usage in the form of nanofluids can make lower dosages (about three times less) than that of the pure drug more effective. Additionally, the expression of the bacterial resistance gene AcrAB decreased, thereby reducing antibiotic resistance and improving drug performance against bacteria.

Keywords: urinary tract infection, antibiotic resistance, carbon nanotube, nanofluid

Procedia PDF Downloads 147

Authors: J. E. Mendes, L. Abrunhosa, J. A. Teixeira, E. R. de Camargo, C. P. de Souza, J. D. C. Pessoa

Abstract:

Among the many promising nanomaterials with antifungal properties, metal nanoparticles (silver nanoparticles) stand out due to their high chemical activity. Therefore, the aim of this study was to evaluate the effect of silver nanoparticles (AgNPs) against Phomopsis sp. AgNPs were synthesized by silver nitrate reduction with sodium citrate and stabilized with ammonia. The synthesized AgNPs have further been characterized by UV/Visible spectroscopy, Biophysical techniques like Dynamic light scattering (DLS) and Scanning Electron Microscopy (SEM). The average diameter of the prepared silver colloidal nanoparticles was about 52 nm. Absolute inhibitions (100%) were observed on treated with a 270 and 540 µg ml-1 concentration of AgNPs. The results from the study of the AgNPs antifungal effect are significant and suggest that the synthesized silver nanoparticles may have an advantage compared with conventional fungicides.

Keywords: antifungal activity, Phomopsis sp., seeds, silver nanoparticles, soybean

Procedia PDF Downloads 463

Authors: Ali Garba Danjani, Abdulrasheed Halliru Usman

Abstract:

Due to the rapidly increasing biological applications and antibacterial properties of versatile chitosan composites, the effects of chitosan/polyvinyl chloride composites film were investigated. Chitosan/polyvinyl chloride films were prepared by a casting method. Polyethylene glycol (PEG) was used as a plasticizer in the blending stage of film preparation. Characterizations of films were done by Scanning Electron microscopy (SEM), Fourier transforms infrared spectroscopy (FTIR), and thermogravimetric analyzer (TGA). Chitosan composites incorporation enhanced the antibacterial activity of chitosan films against Escherichia coli and Staphylococcus aureus. The composite film produced is proposed as packaging or coating material because of its flexibility, antibacterial efficacy, and good mechanical strength.

Keywords: chitosan, polymeric nanocomposites, antibacterial activity, polymer blend

Procedia PDF Downloads 100

Authors: Reem M. Altuwirqi, Mohja S. Summan, Entesar A. Ganash, Safia H. Hamidalddin, Tamer E. Youssef, Mohammed A. Gondal

Abstract:

Laser-Induced Breakdown Spectroscopy (LIBS) technique using 1064 nm Nd: YAG laser was optimized and applied for investigating the existence of radioactive elements (uranium) in twenty-six different ceramic tiles. These tiles were collected from the local Saudi market. Qualitative and quantitative analysis for trace radioactive elements like uranium in these samples was achieved using LIBS. The plasma parameters such as temperature and electron density were calculated to confirm that the plasma generated by the tile samples under laser irradiation can be related to analyte concentrations. In order to perform a quantitative analysis, calibration curves were constructed for two uranium lines (U II (424.166 nm) and U II (424.437 nm)). The Uranium activity concentration in Bq/kg for each sample was measured. Cross-validation of LIBS results with a conventional technique such as Gamma-Ray spectroscopy was also carried out for five ceramic samples. The results show that the LIBS method is an effective way of determining radioactive elements such as uranium in ceramic tiles. Moreover, the uranium concentrations of the investigated samples were below the permissible safe limit for building materials in the majority of samples. Such LIBS system could be applied to determine the presence of natural radioactive elements in ceramic tiles and their radioactivity level rapidly to ensure that they are under the safe allowed limit.

Keywords: laser-induced breakdown spectroscopy, gamma-ray spectroscopy, natural radioactivity, uranium, ceramic tiles

Procedia PDF Downloads 173

Authors: Zafar Mahmood, Fahimullah Babar, Surriyia Naz, Hafiz Ur Rehman

Abstract:

Cadmium Sulphide (CdS) was deposited on a Tec 15 glass substrate with the help of CBD (chemical bath deposition process) and then cadmium telluride CdTe was deposited on CdS with the help of CSS (closed spaced sublimation technique) for the construction of a solar cell. The thicknesses of all the deposited materials were measured with the help of Elipsometry. The IV graphs were drawn in order to observe the current voltage output. The efficiency of the cell was graphed with the fill factor as well (graphs not given here).The efficiency came out to be approximately 16.5 % and the CIGS (copper- indium –gallium- selenide) maximum efficiency is 20 %.The efficiency of a solar cell can further be enhanced by adapting quality materials, good experimental devices and proper procedures. The grain size was analyzed with the help of scanning electron microscope using RBS (Rutherford backscattering spectroscopy).

Keywords: CBD, CdS, CdTe, CSS

Procedia PDF Downloads 364