Search results for: electron microscopy (SEM/TEM)
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 2993

Search results for: electron microscopy (SEM/TEM)

1403 Synthesis, Characterization, Theoretical Crystal Structures and Antitubercular Activity Study of (E)-N'-(2,4-Dihydroxybenzylidene) Nicotinohydrazide and Some of Its Metal Complexes

Authors: Ogunniran Kehinde Olurotimi, Adekoya Joseph, Ehi-Eromosele Cyril, Mehdi Shihab, Mesubi Adediran, Tadigoppula Narender

Abstract:

Nicotinic acid hydrazide and 2,4-dihydoxylbenzaldehyde were condensed at 20°C to form an acylhydrazone (H3L) with ONO coordination pattern. The structure of the acylhydrazone was elucidated by using CHN analyzer, ESI mass spectrometry, IR, 1H NMR, 13C NMR and 2D NMR such as COSY and HSQC. Thereafter, five novel metal complexes [Mn(II), Fe(II), Pt(II) Zn(II) and Pd(II)] of the hydrazone ligand were synthesized and their structural characterization were achieved by several physicochemical methods, namely elemental analysis, electronic spectra, infrared, EPR, molar conductivity and powder X-ray diffraction studies. Structural geometries of some of the compounds were supported by using Hyper Chem-8 program for the molecular mechanics and semi-empirical calculations. The stability energy (E) and electron potentials (eV) for the frontier molecules were calculated by using PM3 method. An octahedral geometry was suggested for both Pd(II) and Zn(II) complexes while both Mn(II) and Fe(II) complexes conformed with tetrahedral pyramidal. However, Pt(II) complex agreed with tetrahedral geometry. In vitro antitubercular activity study of the ligand and the metal complexes were evaluated against Mycobacterium tuberculosis, H37Rv, by using micro-diluted method. The results obtained revealed that (PtL1) (MIC = 0.56 µg/mL), (ZnL1) (MIC = 0.61 µg/mL), (MnL1) (MIC = 0.71 µg/mL) and (FeL1) (MIC = 0.82 µg/mL), exhibited a significant activity when compared with first line drugs such as isoniazid (INH) (MIC = 0.9 µg/mL). H3L1 exhibited lesser antitubercular activity with MIC value of 1.02 µg/mL. However, the metal complexes displayed higher cytoxicity but were found to be non-significant different (P ˂ 0.05) to isoniazid drug.

Keywords: hydrazones, electron spin resonance, thermogravimetric, powder X-ray diffraction, antitubercular agents

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1402 Image Processing of Scanning Electron Microscope Micrograph of Ferrite and Pearlite Steel for Recognition of Micro-Constituents

Authors: Subir Gupta, Subhas Ganguly

Abstract:

In this paper, we demonstrate the new area of application of image processing in metallurgical images to develop the more opportunity for structure-property correlation based approaches of alloy design. The present exercise focuses on the development of image processing tools suitable for phrase segmentation, grain boundary detection and recognition of micro-constituents in SEM micrographs of ferrite and pearlite steels. A comprehensive data of micrographs have been experimentally developed encompassing the variation of ferrite and pearlite volume fractions and taking images at different magnification (500X, 1000X, 15000X, 2000X, 3000X and 5000X) under scanning electron microscope. The variation in the volume fraction has been achieved using four different plain carbon steel containing 0.1, 0.22, 0.35 and 0.48 wt% C heat treated under annealing and normalizing treatments. The obtained data pool of micrographs arbitrarily divided into two parts to developing training and testing sets of micrographs. The statistical recognition features for ferrite and pearlite constituents have been developed by learning from training set of micrographs. The obtained features for microstructure pattern recognition are applied to test set of micrographs. The analysis of the result shows that the developed strategy can successfully detect the micro constitutes across the wide range of magnification and variation of volume fractions of the constituents in the structure with an accuracy of about +/- 5%.

Keywords: SEM micrograph, metallurgical image processing, ferrite pearlite steel, microstructure

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1401 A Modified QuEChERS Method Using Activated Carbon Fibers as r-DSPE Sorbent for Sample Cleanup: Application to Pesticides Residues Analysis in Food Commodities Using GC-MS/MS

Authors: Anshuman Srivastava, Shiv Singh, Sheelendra Pratap Singh

Abstract:

A simple, sensitive and effective gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed for simultaneous analysis of multi pesticide residues (organophosphate, organochlorines, synthetic pyrethroids and herbicides) in food commodities using phenolic resin based activated carbon fibers (ACFs) as reversed-dispersive solid phase extraction (r-DSPE) sorbent in modified QuEChERS (Quick Easy Cheap Effective Rugged Safe) method. The acetonitrile-based QuEChERS technique was used for the extraction of the analytes from food matrices followed by sample cleanup with ACFs instead of traditionally used primary secondary amine (PSA). Different physico-chemical characterization techniques such as Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and Brunauer-Emmet-Teller surface area analysis were employed to investigate the engineering and structural properties of ACFs. The recovery of pesticides and herbicides was tested at concentration levels of 0.02 and 0.2 mg/kg in different commodities such as cauliflower, cucumber, banana, apple, wheat and black gram. The recoveries of all twenty-six pesticides and herbicides were found in acceptable limit (70-120%) according to SANCO guideline with relative standard deviation value < 15%. The limit of detection and limit of quantification of the method was in the range of 0.38-3.69 ng/mL and 1.26 -12.19 ng/mL, respectively. In traditional QuEChERS method, PSA used as r-DSPE sorbent plays a vital role in sample clean-up process and demonstrates good recoveries for multiclass pesticides. This study reports that ACFs are better in terms of removal of co-extractives in comparison of PSA without compromising the recoveries of multi pesticides from food matrices. Further, ACF replaces the need of charcoal in addition to the PSA from traditional QuEChERS method which is used to remove pigments. The developed method will be cost effective because the ACFs are significantly cheaper than the PSA. So the proposed modified QuEChERS method is more robust, effective and has better sample cleanup efficiency for multiclass multi pesticide residues analysis in different food matrices such as vegetables, grains and fruits.

Keywords: QuEChERS, activated carbon fibers, primary secondary amine, pesticides, sample preparation, carbon nanomaterials

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1400 Evaluation of Corrosion Behaviour of Austenitic Steel 08Cr18Ni10Ti Exposed to Supercritical Water

Authors: Monika Šípová, Daniela Marušáková, Claudia Aparicio

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New sources and ways of producing energy are still seeking, and one of the sustainable ways is Generation IV nuclear reactors. The supercritical water-cooled reactor is one of the six nuclear reactors of Generation IV, and as a consequence of the development of light water, reactors seem to be the most perspective. Thus, materials usually used in light water reactors are also tested under the expected operating conditions of the supercritical water-cooled reactor. Austenitic stainless steel 08Cr18Ni10Ti is widely used in the eastern types of light water nuclear power plants. Therefore, specimens of 08Cr18Ni10Ti were exposed to conditions close to the pseudo-critical point of water and high-temperature supercritical water. The description and evaluation of the corrosion behaviour of austenitic stainless steel have been done based on the results of X-ray diffraction in combination with energy dispersive spectroscopy and electron backscatter diffraction. Thus, significant differences have been found in the structure and composition of oxides formed depending on the temperature of exposure. The high temperature of supercritical water resulted in localised form of corrosion in contrast to the thin oxide layer of 1 µm present on the surface of specimens exposed close to the pseudo-critical point of water. The obtained results are important for further research as the supercritical water can be successfully used as a coolant for small modular reactors, which are currently of interest.

Keywords: localised corrosion, supercritical water, stainless steel, electron backscatter diffraction

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1399 Altering Surface Properties of Magnetic Nanoparticles with Single-Step Surface Modification with Various Surface Active Agents

Authors: Krupali Mehta, Sandip Bhatt, Umesh Trivedi, Bhavesh Bharatiya, Mukesh Ranjan, Atindra D. Shukla

Abstract:

Owing to the dominating surface forces and large-scale surface interactions, the nano-scale particles face difficulties in getting suspended in various media. Magnetic nanoparticles of iron oxide offer a great deal of promise due to their ease of preparation, reasonable magnetic properties, low cost and environmental compatibility. We intend to modify the surface of magnetic Fe₂O₃ nanoparticles with selected surface modifying agents using simple and effective single-step chemical reactions in order to enhance dispersibility of magnetic nanoparticles in non-polar media. Magnetic particles were prepared by hydrolysis of Fe²⁺/Fe³⁺ chlorides and their subsequent oxidation in aqueous medium. The dried particles were then treated with Octadecyl quaternary ammonium silane (Terrasil™), stearic acid and gallic acid ester of stearyl alcohol in ethanol separately to yield S-2 to S-4 respectively. The untreated Fe₂O₃ was designated as S-1. The surface modified nanoparticles were then analysed with Dynamic Light Scattering (DLS), Fourier Transform Infrared spectroscopy (FTIR), X-Ray Diffraction (XRD), Thermogravimetric Gravimetric Analysis (TGA) and Scanning Electron Microscopy and Energy dispersive X-Ray analysis (SEM-EDAX). Characterization reveals the particle size averaging 20-50 nm with and without modification. However, the crystallite size in all cases remained ~7.0 nm with the diffractogram matching to Fe₂O₃ crystal structure. FT-IR suggested the presence of surfactants on nanoparticles’ surface, also confirmed by SEM-EDAX where mapping of elements proved their presence. TGA indicated the weight losses in S-2 to S-4 at 300°C onwards suggesting the presence of organic moiety. Hydrophobic character of modified surfaces was confirmed with contact angle analysis, all modified nanoparticles showed super hydrophobic behaviour with average contact angles ~129° for S-2, ~139.5° for S-3 and ~151° for S-4. This indicated that surface modified particles are super hydrophobic and they are easily dispersible in non-polar media. These modified particles could be ideal candidates to be suspended in oil-based fluids, polymer matrices, etc. We are pursuing elaborate suspension/sedimentation studies of these particles in various oils to establish this conjecture.

Keywords: iron nanoparticles, modification, hydrophobic, dispersion

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1398 Ultrastructural Changes Occur in Mice Lungs After Cessation to Exposure of Incense Smoke

Authors: Samar Rabah

Abstract:

Background: Incense woods are special kind of trees called Agarwood, which characterized by good smelling odors and many medical benefits. Incense smoke is heavily used in Saudi Arabia although comprehensive studies of its effects on health are limited. The present study demonstrated lung ultrastructure changes of mice after exposure and cessation to Incense smoke. Eighty mice are divided equally into four groups, three groups are exposed to different concentrations of Incense smoke (2, 4 and 6 gm) for three months, while the fourth group is control one. At the end of each month, lungs of five animals from each group are gathered, while the last five animals from each group are kept for another 60 days without exposure to the Incense smoke to allow for recovery. Results: Transmission electron microscope investigations of all exposed groups showed hypertrophy and hyperplasia in Clara Cells and some an enlargement of the macrophage to the point that it fills a large part of the alveolar lumen. Scanning electron microscope marks presence of mucus materials attached to the epithelial bronchioles. After prevention of exposure to the Incense smoke for 60 days, necrosis and degeneration in some cells of epithelial bronchioles, fibrosis of peribronchial, thickening in alveolar walls and aggregation of lymphoid cells were demonstrated. Conclusion: Based on the above findings and other related studies (not published), we conclude that exposure to Incense smoke causes harmful effects due to sever changes in pulmonary ultrastructure, such effects do not disappear even when Incense smoke inhalation was stopped. Therefore, we recommend that Incense smoke should use only in open places to reduce its harms.

Keywords: Incense smoke, lungs, ultrastructure of lungs, Agarwood

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1397 Electromagnetic Interface Shielding of Graphene Oxide–Carbon Nanotube Hybrid ABS Composites

Authors: Jeevan Jyoti, Bhanu Pratap Singh, S. R. Dhakate

Abstract:

In the present study, multiwalled carbon nanotubes (MWCNTs) and reduced graphene oxide (RGO) were synthesized by chemical vapor deposition and Improved Hummer’s method, respectively and their composite with acrylonitrile butadiene styrene (ABS) were prepared by twin screw co rotating extrusion technique. The electromagnetic interference (EMI) shielding effectiveness of graphene oxide carbon nanotube (GCNTs) hybrid composites was investigated and the results were compared with EMI shielding of carbon nanotube (CNTs) and reduced graphene oxide (RGO) in the frequency range of 12.4-18 GHz (Ku-band). The experimental results indicate that the EMI shielding effectiveness of these composites is achieved up to –21 dB for 10 wt. % loading of GCNT loading. The mechanism of improvement in EMI shielding effectiveness is discussed by resolving their contribution in absorption and reflection loss. The main reason for such a high improved shielding effectiveness has been attributed to the significant improvement in the electrical conductivity of the composites. The electrical conductivity of these GCNT/ABS composites was increased from 10-13 S/cm to 10-7 S/cm showing the improvement of the 6 order of the magnitude. Scanning electron microscopic (SEM) and high resolution transmission electron microscopic (HRTEM) studies showed that the GCNTs were uniformly dispersed in the ABS polymer matrix. GCNTs form a network throughout the polymer matrix and promote the reinforcement.

Keywords: ABS, EMI shielding, multiwalled carbon nanotubes, reduced graphene oxide, graphene, oxide-carbon nanotube (GCNTs), twin screw extruder, multiwall carbon nanotube, electrical conductivity

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1396 Late Bronze Age Pigments: Characterization of Mycenaean Pottery with Multi-Analytical Approach

Authors: Elif Doğru, Bülent Kızılduman, Huriye İcil

Abstract:

Throughout history, Cyprus has been involved in various commercial and cultural relationships with different civilizations, owing to its strategic location. Particularly during the Late Bronze Age, Cyprus emerged as a significant region engaged in interactions with the Mycenaeans and other Mediterranean civilizations. Presently, findings from archaeological excavations provide valuable insights into Cyprus' cultural history and its connections with other civilizations. Painted Mycenaean ceramics discovered during the excavations at Kaleburnu-Kral Tepesi (Galinaporni-Vasili), dated to the Late Bronze Age in Cyprus, are considered significant archaeological findings that carry traces of the art and culture of that era, reflecting the island's commercial and cultural connections. Considering these findings, there is a need for archaeometric studies to aid in the understanding of the commercial and cultural ties at Kaleburnu-Kral Tepesi. In line with this need, analytical studies have been initiated concerning the provenance and production techniques of the Mycenaean ceramics discovered in the excavations at Kaleburnu-Kral Tepesi, dated to the Late Bronze Age. In the context of origin analysis studies, it is advocated that understanding the techniques and materials used for the figures and designs applied on Mycenaean ceramics would significantly contribute to a better comprehension of historical contexts. Hence, the adopted approach involves not only the analysis of the ceramic raw material but also the characterization of the pigments on the ceramics as a whole. In light of this, in addition to the studies aimed at determining the provenance and production techniques of the Mycenaean ceramic bodies, the characterization of the pigments used in the decorations of the relevant ceramics has been included in the research scope. Accordingly, this study aims to characterize the pigments used in the decorations of Mycenaean ceramics discovered at Kaleburnu-Kral Tepesi, dated to the Late Bronze Age. The X-Ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM-EDX) methods have been employed to determine the surface morphology and chemical properties of the Mycenaean pigments. The characterization has been conducted through the combination of multiple analytical methods. The characterization of the pigments of Mycenaean ceramics aims to enhance the scientific perspective adopted for understanding the contributions of Mycenaean ceramics found in Cyprus to the island's culture, by providing scientific data on the types and origins of pigments used during the Late Bronze Age.

Keywords: mycenaean, ceramic, provenance, pigment

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1395 Amino Acid Based Biodegradable Poly (Ester-Amide)s and Their Potential Biomedical Applications as Drug Delivery Containers and Antibacterial

Authors: Nino Kupatadze, Tamar Memanishvili, Natia Ochkhikidze, David Tugushi, Zaal Kokaia, Ramaz Katsarava

Abstract:

Amino acid-based Biodegradable poly(ester-amide)s (PEAs) have gained considerable interest as a promising materials for numerous biomedical applications. These polymers reveal a high biocompatibility and easily form small particles suitable for delivery various biological, as well as elastic bio-erodible films serving as matrices for constructing antibacterial coatings. In the present work we have demonstrated a potential of the PEAs for two applications: 1. cell therapy for stroke as vehicles for delivery and sustained release of growth factors, 2. bactericidal coating as prevention biofilm and applicable in infected wound management. Stroke remains the main cause of adult disability with limited treatment options. Although stem cell therapy is a promising strategy, it still requires improvement of cell survival, differentiation and tissue modulation. .Recently, microspheres (MPs) made of biodegradable polymers have gained significant attention for providing necessary support of transplanted cells. To investigate this strategy in the cell therapy of stroke, MPs loaded with transcription factors Wnt3A/BMP4 were prepared. These proteins have been shown to mediate the maturation of the cortical neurons. We have suggested that implantation of these materials could create a suitable microenvironment for implanted cells. Particles with spherical shape, porous surface, and 5-40 m in size (monitored by scanning electron microscopy) were made on the basis of the original PEA composed of adipic acid, L-phenylalanine and 1,4-butanediol. After 4 months transplantation of MPs in rodent brain, no inflammation was observed. Additionally, factors were successfully released from MPs and affected neuronal cell differentiation in in vitro. The in vivo study using loaded MPs is in progress. Another severe problem in biomedicine is prevention of surgical devices from biofilm formation. Antimicrobial polymeric coatings are most effective “shields” to protect surfaces/devices from biofilm formation. Among matrices for constructing the coatings preference should be given to bio-erodible polymers. Such types of coatings will play a role of “unstable seating” that will not allow bacteria to occupy the surface. In other words, bio-erodible coatings would be discomfort shelter for bacteria that along with releasing “killers of bacteria” should prevent the formation of biofilm. For this purpose, we selected an original biodegradable PEA composed of L-leucine, 1,6-hexanediol and sebacic acid as a bio-erodible matrix, and nanosilver (AgNPs) as a bactericidal agent (“killer of bacteria”). Such nanocomposite material is also promising in treatment of superficial wound and ulcer. The solubility of the PEA in ethanol allows to reduce AgNO3 to NPs directly in the solution, where the solvent served as a reductive agent, and the PEA served as NPs stabilizer. The photochemical reduction was selected as a basic method to form NPs. The obtained AgNPs were characterized by UV-spectroscopy, transmission electron microscope (TEM), and dynamic light scattering (DLS). According to the UV-data and TEM data the photochemical reduction resulted in spherical AgNPs with wide particle size distribution with a high contribution of the particles below 10 nm that are known as responsible for bactericidal activity of AgNPs. DLS study showed that average size of nanoparticles formed after photo-reduction in ethanol solution ranged within ca. 50 nm.

Keywords: biodegradable polymers, microparticles, nanocomposites, stem cell therapy, stroke

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1394 Mesocarbon Microbeads Modification of Stainless-Steel Current Collector to Stabilize Lithium Deposition and Improve the Electrochemical Performance of Anode Solid-State Lithium Hybrid Battery

Authors: Abebe Taye

Abstract:

The interest in enhancing the performance of all-solid-state batteries featuring lithium metal anodes as a potential alternative to traditional lithium-ion batteries has prompted exploration into new avenues. A promising strategy involves transforming lithium-ion batteries into hybrid configurations by integrating lithium-ion and lithium-metal solid-state components. This study is focused on achieving stable lithium deposition and advancing the electrochemical capabilities of solid-state lithium hybrid batteries with anodes by incorporating mesocarbon microbeads (MCMBs) blended with silver nanoparticles. To achieve this, mesocarbon microbeads (MCMBs) blended with silver nanoparticles are coated on stainless-steel current collectors. These samples undergo a battery of analyses employing diverse techniques. Surface morphology is studied through scanning electron microscopy (SEM). The electrochemical behavior of the coated samples is evaluated in both half-cell and full-cell setups utilizing an argyrodite-type sulfide electrolyte. The stability of MCMBs in the electrolyte is assessed using electrochemical impedance spectroscopy (EIS). Additional insights into the composition are gleaned through X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). At an ultra-low N/P ratio of 0.26, stability is upheld for over 100 charge/discharge cycles in half-cells. When applied in a full-cell configuration, the hybrid anode preserves 60.1% of its capacity after 80 cycles at 0.3 C under a low N/P ratio of 0.45. In sharp contrast, the capacity retention of the cell using untreated MCMBs declines to 20.2% after a mere 60 cycles. The introduction of mesocarbon microbeads (MCMBs) combined with silver nanoparticles into the hybrid anode of solid-state lithium batteries substantially elevates their stability and electrochemical performance. This approach ensures consistent lithium deposition and removal, mitigating dendrite growth and the accumulation of inactive lithium. The findings from this investigation hold significant value in elevating the reversibility and energy density of lithium-ion batteries, thereby making noteworthy contributions to the advancement of more efficient energy storage systems.

Keywords: MCMB, lithium metal, hybrid anode, silver nanoparticle, cycling stability

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1393 Nanomaterials for Archaeological Stone Conservation: Re-Assembly of Archaeological Heavy Stones Using Epoxy Resin Modified with Clay Nanoparticles

Authors: Sayed Mansour, Mohammad Aldoasri, Nagib Elmarzugi, Nadia A. Al-Mouallimi

Abstract:

The archaeological large stone used in construction of ancient Pharaonic tombs, temples, obelisks and other sculptures, always subject to physicomechanical deterioration and destructive forces, leading to their partial or total broken. The task of reassembling this type of artifact represent a big challenge for the conservators. Recently, the researchers are turning to new technologies to improve the properties of traditional adhesive materials and techniques used in re-assembly of broken large stone. The epoxy resins are used extensively in stone conservation and re-assembly of broken stone because of their outstanding mechanical properties. The introduction of nanoparticles to polymeric adhesives at low percentages may lead to substantial improvements of their mechanical performances in structural joints and large objects. The aim of this study is to evaluate the effectiveness of clay nanoparticles in enhancing the performances of epoxy adhesives used in re-assembly of archaeological massive stone by adding proper amounts of those nanoparticles. The nanoparticles reinforced epoxy nanocomposite was prepared by direct melt mixing with a nanoparticles content of 3% (w/v), and then mould forming in the form of rectangular samples, and used as adhesive for experimental stone samples. Scanning electron microscopy (SEM) was employed to investigate the morphology of the prepared nanocomposites, and the distribution of nanoparticles inside the composites. The stability and efficiency of the prepared epoxy-nanocomposites and stone block assemblies with new formulated adhesives were tested by aging artificially the samples under different environmental conditions. The effect of incorporating clay nanoparticles on the mechanical properties of epoxy adhesives was evaluated comparatively before and after aging by measuring the tensile, compressive, and Elongation strength tests. The morphological studies revealed that the mixture process between epoxy and nanoparticles has succeeded with a relatively homogeneous morphology and good dispersion in low nano-particles loadings in epoxy matrix was obtained. The results show that the epoxy-clay nanocomposites exhibited superior tensile, compressive, and Elongation strength. Moreover, a marked improvement of the mechanical properties of stone joints increased in all states by adding nano-clay to epoxy in comparison with pure epoxy resin.

Keywords: epoxy resins, nanocomposites, clay nanoparticles, re-assembly, archaeological massive stones, mechanical properties

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1392 Optical Emission Studies of Laser Produced Lead Plasma: Measurements of Transition Probabilities of the 6P7S → 6P2 Transitions Array

Authors: Javed Iqbal, R. Ahmed, M. A. Baig

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We present new data on the optical emission spectra of the laser produced lead plasma using a pulsed Nd:YAG laser at 1064 nm (pulse energy 400 mJ, pulse width 5 ns, 10 Hz repetition rate) in conjunction with a set of miniature spectrometers covering the spectral range from 200 nm to 720 nm. Well resolved structure due to the 6p7s → 6p2 transition array of neutral lead and a few multiplets of singly ionized lead have been observed. The electron temperatures have been calculated in the range (9000 - 10800) ± 500 K using four methods; two line ratio, Boltzmann plot, Saha-Boltzmann plot and Morrata method whereas, the electron number densities have been determined in the range (2.0 – 8.0) ± 0.6 ×1016 cm-3 using the Stark broadened line profiles of neutral lead lines, singly ionized lead lines and hydrogen Hα-line. Full width at half maximum (FWHM) of a number of neutral and singly ionized lead lines have been extracted by the Lorentzian fit to the experimentally observed line profiles. Furthermore, branching fractions have been deduced for eleven lines of the 6p7s → 6p2 transition array in lead whereas the absolute values of the transition probabilities have been calculated by combining the experimental branching fractions with the life times of the excited levels The new results are compared with the existing data showing a good agreement.

Keywords: LIBS, plasma parameters, transition probabilities, branching fractions, stark width

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1391 Durability of Functionally Graded Concrete

Authors: Prasanna Kumar Acharya, Mausam Kumari Yadav

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Cement concrete has emerged as the most consumed construction material. It has also dominated all other construction materials because of its versatility. Apart from numerous advantages it has a disadvantage concerning durability. The large structures constructed with cement concrete involving the consumption of huge natural materials remain in serviceable condition for 5 – 7 decades only while structures made with stones stand for many centuries. The short life span of structures not only affects the economy but also affects the ecology greatly. As such, the improvement of durability of cement concrete is a global concern and scientists around the globe are trying for this purpose. Functionally graded concrete (FGC) is an exciting development. In contrast to conventional concrete, FGC demonstrates different characteristics depending on its thickness, which enables it to conform to particular structural specifications. The purpose of FGC is to improve the performance and longevity of conventional concrete structures with cutting-edge building materials. By carefully distributing various kinds and amounts of reinforcements, additives, mix designs and/or aggregates throughout the concrete matrix, this variety is produced. A key component of functionally graded concrete's performance is its durability, which affects the material's capacity to tolerate aggressive environmental influences and load-bearing circumstances. This paper reports the durability of FGC made using Portland slag cement (PSC). For this purpose, control concretes (CC) of M20, M30 and M40 grades were designed. Single-layered samples were prepared using each grade of concrete. Further using combinations of M20 + M30, M30 + M40 and M40 + M20, doubled layered concrete samples in a depth ratio of 1:1 was prepared those are herein called FGC samples. The efficiency of FGC samples was compared with that of the higher-grade concrete of parent materials in terms of compressive strength, water absorption, sorptivity, acid resistance, sulphate resistance, chloride resistance and abrasion resistance. The properties were checked at the age of 28 and 91 days. Apart from strength and durability parameters, the microstructure of CC and FGC were studied in terms of X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray. The result of the study revealed that there is an increase in the efficiency of concrete evaluated in terms of strength and durability when it is made functionally graded using a layered technology having different grades of concrete in layers. The results may help to enhance the efficiency of structural concrete and its durability.

Keywords: fresh on compacted, functionally graded concrete, acid, chloride, sulphate test, sorptivity, abrasion, water absorption test

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1390 Evaluation of the Effect of Magnetic Field on Fibroblast Attachment in Contact with PHB/Iron Oxide Nanocomposite

Authors: Shokooh Moghadam, Mohammad Taghi Khorasani, Sajjad Seifi Mofarah, M. Daliri

Abstract:

Through the recent two decades, the use of magnetic-property materials with the aim of target cell’s separation and eventually cancer treatment has incredibly increased. Numerous factors can alter the efficacy of this method on curing. In this project, the effect of magnetic field on adhesion of PDL and L929 cells on nanocomposite of iron oxide/PHB with different density of iron oxides (1%, 2.5%, 5%) has been studied. The nanocamposite mentioned includes a polymeric film of poly hydroxyl butyrate and γ-Fe2O3 particles with the average size of 25 nanometer dispersed in it and during this process, poly vinyl alcohol with 98% hydrolyzed and 78000 molecular weight was used as an emulsion to achieve uniform distribution. In order to get the homogenous film, the solution of PHB and iron oxide nanoparticles were put in a dry freezer and in liquid nitrogen, which resulted in a uniform porous scaffold and for removing porosities a 100◦C press was used. After the synthesis of a desirable nanocomposite film, many different tests were performed, First, the particles size and their distribution in the film were evaluated by transmission electron microscopy (TEM) and even FTIR analysis and DMTA test were run in order to observe and accredit the chemical connections and mechanical properties of nanocomposites respectively. By comparing the graphs of case and control samples, it was established that adding nano particles caused an increase in crystallization temperature and the more density of γ-Fe2O3 lead to more Tg (glass temperature). Furthermore, its dispersion range and dumping property of samples were raised up. Moreover, the toxicity, morphologic changes and adhesion of fibroblast and cancer cells were evaluated by a variety of tests. All samples were grown in different density and in contact with cells for 24 and 48 hours within the magnetic fields of 2×10^-3 Tesla. After 48 hours, the samples were photographed with an optic and SEM and no sign of toxicity was traced. The number of cancer cells in the case of sample group was fairly more than the control group. However, there are many gaps and unclear aspects to use magnetic field and their effects in cancer and all diseases treatments yet to be discovered, not to neglect that there have been prominent step on this way in these recent years and we hope this project can be at least a minimum movement in this issue.

Keywords: nanocomposite, cell attachment, magnetic field, cytotoxicity

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1389 The Effect of Organic Matter Maturation and Porosity Evolution on Methane Storage Potential in Shale-Gas Reservoirs

Authors: T. Topór, A. Derkowski, P. Ziemiański

Abstract:

Formation of organic matter (OM)-hosted nanopores upon thermal maturation are one of the key factor controlling methane storage potential in unconventional shale-gas reservoirs. In this study, the subcritical CO₂ and N₂ gas adsorption measurements combined with scanning electron microscopy and supercritical methane adsorption have been used to characterize pore system and methane storage potential in black shales from the Baltic Basin (Poland). The samples were collected from a virtually equivalent Llandovery strata across the basin and represent a complete digenetic sequence, from thermally immature to overmature. The results demonstrate that the thermal maturation is a dominant mechanism controlling the formation of OM micro- and mesopores in the Baltic Basin shales. The formation of micro- and mesopores occurs in the oil window (vitrinite reflectance; leavedVR; ~0.5-0.9%) as a result of oil expulsion from kerogenleft OM highly porous. The generated hydrocarbons then turn into solid bitumen causing pore blocking and substantial decrease in micro- and mesopore volume in late-mature shales (VR ~0.9-1.2%). Both micro- and mesopores are regenerated in a middle of the catagenesis range (VR 1.4-1.9%) due to secondary cracking of OM and gas formation. The micropore volume in investigated shales is almost exclusively controlled by the OM content. The contribution of clay minerals to micropore volume is insignificant and masked by a strong contribution from OM. Methane adsorption capacity in the Baltic Basin shales is predominantly controlled by microporous OM with pores < 1.5 nm. The mesopore volume (2-50 nm) and mesopore surface area have no effect on methane sorption behavior. The adsorbed methane density equivalent, calculated as absolute methane adsorption divided by micropore volume, reviled a decrease of the methane loading potential in micropores with increasing maturity. The highest methane loading potential in micropores is observed for OM before metagenesis (VR < 2%), where the adsorbed methane density equivalent is greater than the density of liquid methane. This implies that, in addition to physical adsorption, absorption of methane in OM may occur before metagenesis. After OM content reduction using NaOCl solution methane adoption capacity substantially decreases, suggesting significantly greater adsorption potential for OM microstructure than for the clay minerals matrix.

Keywords: maturation, methane sorption, organic matter, porosity, shales

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1388 Extraction of Scandium (Sc) from an Ore with Functionalized Nanoporous Silicon Adsorbent

Authors: Arezoo Rahmani, Rinez Thapa, Juha-Matti Aalto, Petri Turhanen, Jouko Vepsalainen, Vesa-PekkaLehto, Joakim Riikonen

Abstract:

Production of Scandium (Sc) is a complicated process because Sc is found only in low concentrations in ores and the concentration of Sc is very low compared with other metals. Therefore, utilization of typical extraction processes such as solvent extraction is problematic in scandium extraction. The Adsorption/desorption method can be used, but it is challenging to prepare materials, which have good selectivity, high adsorption capacity, and high stability. Therefore, efficient and environmentally friendly methods for Sc extraction are needed. In this study, the nanoporous composite material was developed for extracting Sc from an Sc ore. The nanoporous composite material offers several advantageous properties such as large surface area, high chemical and mechanical stability, fast diffusion of the metals in the material and possibility to construct a filter out of the material with good flow-through properties. The nanoporous silicon material was produced by first stabilizing the surfaces with a silicon carbide layer and then functionalizing the surface with bisphosphonates that act as metal chelators. The surface area and porosity of the material were characterized by N₂ adsorption and the morphology was studied by scanning electron microscopy (SEM). The bisphosphonate content of the material was studied by thermogravimetric analysis (TGA). The concentration of metal ions in the adsorption/desorption experiments was measured with inductively coupled plasma mass spectrometry (ICP-MS). The maximum capacity of the material was 25 µmol/g Sc at pH=1 and 45 µmol/g Sc at pH=3, obtained from adsorption isotherm. The selectivity of the material towards Sc in artificial solutions containing several metal ions was studied at pH one and pH 3. The result shows good selectivity of the nanoporous composite towards adsorption of Sc. Scandium was less efficiently adsorbed from solution leached from the ore of Sc because of excessive amounts of iron (Fe), aluminum (Al) and titanium (Ti) which disturbed the adsorption process. For example, the concentration of Fe was more than 4500 ppm, while the concentration of Sc was only three ppm, approximately 1500 times lower. Precipitation methods were developed to lower the concentration of the metals other than Sc. Optimal pH for precipitation was found to be pH 4. The concentration of Fe, Al and Ti were decreased by 99, 70, 99.6%, respectively, while the concentration of Sc decreased only 22%. Despite the large reduction in the concentration of other metals, more work is needed to further increase the relative concentration of Sc compared with other metals to efficiently extract it using the developed nanoporous composite material. Nevertheless, the developed material may provide an affordable, efficient and environmentally friendly method to extract Sc on a large scale.

Keywords: adsorption, nanoporous silicon, ore solution, scandium

Procedia PDF Downloads 146
1387 Dimensionality Control of Li Transport by MOFs Based Quasi-Solid to Solid Electrolyte

Authors: Manuel Salado, Mikel Rincón, Arkaitz Fidalgo, Roberto Fernandez, Senentxu Lanceros-Méndez

Abstract:

Lithium-ion batteries (LIBs) are a promising technology for energy storage, but they suffer from safety concerns due to the use of flammable organic solvents in their liquid electrolytes. Solid-state electrolytes (SSEs) offer a potential solution to this problem, but they have their own limitations, such as poor ionic conductivity and high interfacial resistance. The aim of this research was to develop a new type of SSE based on metal-organic frameworks (MOFs) and ionic liquids (ILs). MOFs are porous materials with high surface area and tunable electronic properties, making them ideal for use in SSEs. ILs are liquid electrolytes that are non-flammable and have high ionic conductivity. A series of MOFs were synthesized, and their electrochemical properties were evaluated. The MOFs were then infiltrated with ILs to form a quasi-solid gel and solid xerogel SSEs. The ionic conductivity, interfacial resistance, and electrochemical performance of the SSEs were characterized. The results showed that the MOF-IL SSEs had significantly higher ionic conductivity and lower interfacial resistance than conventional SSEs. The SSEs also exhibited excellent electrochemical performance, with high discharge capacity and long cycle life. The development of MOF-IL SSEs represents a significant advance in the field of solid-state electrolytes. The high ionic conductivity and low interfacial resistance of the SSEs make them promising candidates for use in next-generation LIBs. The data for this research was collected using a variety of methods, including X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopy. The data was analyzed using a variety of statistical and computational methods, including principal component analysis, density functional theory, and molecular dynamics simulations. The main question addressed by this research was whether MOF-IL SSEs could be developed that have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. The results of this research demonstrate that MOF-IL SSEs are a promising new type of solid-state electrolyte for use in LIBs. The SSEs have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. These properties make them promising candidates for use in next-generation LIBs that are safer and have higher energy densities.

Keywords: energy storage, solid-electrolyte, ionic liquid, metal-organic-framework, electrochemistry, organic inorganic plastic crystal

Procedia PDF Downloads 83
1386 Doped TiO2 Thin Films Microstructural and Electrical Properties

Authors: Mantas Sriubas, Kristina Bockute, Darius Virbukas, Giedrius Laukaitis

Abstract:

In this work, the doped TiO2 (dopants – Ca, Mg) was investigated. The comparison between the physical vapour deposition methods as electron beam vapour deposition and magnetron sputtering was performed and the structural and electrical properties of the formed thin films were investigated. Thin films were deposited on different type of substrates: SiO2, Alloy 600 (Fe-Ni-Cr) and Al2O3 substrates. The structural properties were investigated using Ambios XP-200 profilometer, scanning electron microscope (SEM) Hitachi S-3400N, X-ray energy-dispersive spectroscope (EDS) Quad 5040 (Bruker AXS Microanalysis GmbH), X-ray diffractometer (XRD) D8 Discover (Bruker AXS GmbH) with glancing angles focusing geometry in a 20 – 70° range using the Cu Kα1 λ = 0.1540562 nm radiation). The impedance spectroscopy measurements were performed using Probostat® (NorECs AS) measurement cell in the frequency range from 10-1-106 Hz under reducing and oxidizing conditions in temperature range of 200 °C to 1200 °C. The investigation of the e-beam deposited Ca and Mg doped-TiO2 thin films shows that the thin films are dense without any visible pores and cavities and the thin films grow in zone T according Barna-Adamik SZM. Substrate temperature was kept 600 °C during the deposition and Ts/Tm ≈ 0.32 (substrate temperature (Ts) and coating material melting temperature (Tm)). The surface diffusion is high however, the grain boundary migration is strongly limited at this temperature. This means that structure is inhomogeneous and the columnar structure is mostly visible in the upper part of the films. According to XRD, the increasing of the Ca dopants’ concentration increases the crystallinity of the formed thin films and the crystallites size increase linearly and Ca dopants act as prohibitors. Thin films are comprised of anatase TiO2 phase with an exception of 2 % Ca doped TiO2, where a small peak of Ca arise. In the case of Mg doped-TiO2 the intensities of the XRD peaks decreases with increasing Mg molar concentration. It means that there are less diffraction planes of the particular orientation in thin films with higher impurities concentration. Thus, the crystallinity decreases with increasing Mg concentration and Mg dopants act as inhibitors. The impedance measurements show that the dopants changed the conductivity of the formed thin films. The conductivity varies from 10-3 S/cm to 10-4 S/cm at 800 °C under wet reducing conditions. The microstructure of the magnetron sputtered thin TiO2 films is different comparing to the thin films deposited using e-beam deposition therefore influencing other structural and electrical properties.

Keywords: electrical properties, electron beam deposition, magnetron sputtering, microstructure, titanium dioxide

Procedia PDF Downloads 297
1385 Depositional Environment and Diagenetic Alterations, Influences of Facies and Fine Kaolinite Formation Migration on Sandstones’ Reservoir Quality, Sarir Formation, Sirt Basin Libya

Authors: Faraj M. Elkhatri, Hana Ali Allafi

Abstract:

The spatial and temporal distribution of diagenetic alterations related impact on the reservoir quality of the Sarir Formation. (present day burial depth of about 9000 feet) Depositional facies and diagenetic alterations are the main controls on reservoir quality of Sarir Formation Sirt Ba-sin Libya; these based on lithology and grain size as well as authigenic clay mineral types and their distributions. However, petrology investigation obtained on study area with five sandstone wells concentrated on main rock components and the parameters that may have impacts on reservoirs. the main authigenic clay minerals are kaolinite and dickite, these investigations have confirmed by X.R.D analysis and clay fraction. mainly Kaolinite and Dickite were extensively presented on all of wells with high amounts. As well as trace of detrital smectite and less amounts of illitized mud-matrix are possibly find by SEM image. Thin layers of clay presented as clay-grain coatings in local depth interpreted as remains of dissolved clay matrix is partly transformed into kaolinite adjacent and towards pore throat. This also may have impacts on most of the pore throats of this sandstone which are open and relatively clean with some of fine martial have been formed on occluded pores. This material is identified by EDS analysis to be collections of not only kaolinite booklets, but also small, disaggregated kaolinite platelets derived from the dis-aggregation of larger kaolinite booklets. These patches of kaolinite not only fill this pore, but also coat some of the sur-rounding framework grains. Quartz grains often enlarged by authigenic quartz overgrowths partially occlude and re-duce porosity. Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM) was conducted on the post-test samples to examine any mud filtrate particles that may be in the pore throats. Semi-qualitative elemental data on select-ed minerals observed during the SEM study were obtained using an Energy Dispersive Spectroscopy (EDS) unit. The samples showed mostly clean open pore throats, with limited occlusion by kaolinite.

Keywords: por throat, formation damage, porosity lose, solids plugging

Procedia PDF Downloads 60
1384 Study on the Mechanical Properties of Bamboo Fiber-Reinforced Polypropylene Based Composites: Effect of Gamma Radiation

Authors: Kamrun N. Keya, Nasrin A. Kona, Ruhul A. Khan

Abstract:

Bamboo fiber (BF) reinforced polypropylene (PP) based composites were fabricated by a conventional compression molding technique. In this investigation, bamboo composites were manufactured using different percentages of fiber, which were varying from 25-65% on the total weight of the composites. To fabricate the BF/PP composites untreated and treated fibers were selected. A systematic study was done to observe the physical, mechanical, and interfacial behavior of the composites. In this study, mechanical properties of the composites such as tensile, impact, and bending properties were observed precisely. Maximum tensile strength (TS) and bending strength (BS) were found for 50 wt% fiber composites, 65 MPa, and 85.5 MPa respectively, whereas the highest tensile modulus (TM) and bending modulus (BM) was examined, 5.73 GPa and 7.85 GPa respectively. The BF/PP based composites were treated with irradiated under gamma radiation (the source strength 50 kCi Cobalt-60) of various doses (i.e. 10, 20, 30, 40, 50 and 60 kGy doses). The effect of gamma radiation on the composites was also investigated, and it found that the effect of 30.0 kGy (i.e. units for radiation measurement is 'gray', kGy=kilogray) gamma dose showed better mechanical properties than other doses. After flexural testing, fracture sides of the untreated and treated both composites were studied by scanning electron microscope (SEM). SEM results of the treated BF/PP based composites showed better fiber-matrix adhesion and interfacial bonding than untreated BF/PP based composites. Water uptake and soil degradation tests of untreated and treated composites were also investigated.

Keywords: bamboo fiber, polypropylene, compression molding technique, gamma radiation, mechanical properties, scanning electron microscope

Procedia PDF Downloads 133
1383 Steps of the Pancreatic Differentiation in the Grass Snake (Natrix natrix) Embryos

Authors: Magdalena Kowalska, Weronika Rupik

Abstract:

The pancreas is an important organ present in all vertebrate species. It contains two different tissues, exocrine and endocrine, that act as two glands in one. The development and differentiation of the pancreas in reptiles is poorly known in comparison to other vertebrates. Therefore, the aim of this study was to investigate the particular steps concerning the differentiation of the pancreas in the grass snake (Natrix natrix) embryos. For this, histological methods (including hematoxylin and eosin, and Heidenhain's AZAN staining), transmission electron microscopy and three-dimensional (3D) reconstructions from serial paraffin sections were used. The results of this study indicated that the first step of pancreas development in Natrix was the connection of the two pancreatic buds: dorsal and ventral one. Then, duct walls in both buds started to be remodeled from the multilayered to single-layered epithelium. This remodeling started in the dorsal bud and was simultaneously with the differentiation of the duct lumens which occurred by the cavition. During this process, the cells that had no contact with the mesenchyme underwent cell death named anoikis. These findings indicated that the walls of ducts in the embryonic pancreas of the grass snake were initially formed by the abundant principal and single endocrine cells. Later the basal and goblet cells differentiated. Among the endocrine cells, as the first the B and A cells differentiated, then the D and PP cells. The next step of the pancreatic development was the withdrawing of the endocrine cells from the duct walls to form the pancreatic islets. The endocrine cells and islets were found only in the dorsal part of the pancreas in Natrix embryos what is different than in other vertebrate species. The islets were formed mainly by the A cells. Simultaneously, with the differentiation of the endocrine pancreas, the acinar tissue started to differentiate. The source of the acinar cells were pancreatic ducts similar as in other vertebrates. The acini formation began at the proximal part of the pancreas and went towards the caudal direction. Differentiating pancreatic ducts developed into the branched system that can be divided into extralobular, intralobular, and intercalated ducts, similarly as in other vertebrate species. However, the pattern of branching was different. In conclusions, particular steps of the pancreas differentiation in the grass snake were different than in other vertebrates. It can be supposed that these differences are related to the specific topography of the snake’s internal organs and their taxonomy position. All specimens used in the study were captured according to the Polish regulations concerning the protection of wild species. Permission was granted by the Local Ethics Commission in Katowice (41/2010; 87/2015) and the Regional Directorate for Environmental Protection in Katowice (WPN.6401.257.2015.DC).

Keywords: embryogenesis, organogenesis, pancreas, Squamata

Procedia PDF Downloads 171
1382 Radiosensitization Properties of Gold Nanoparticles in Brachytherapy of Uterus Cancer by High Dose Rate I-125 Seed: A Simulation Study by MCNPX and MCNP6 Codes

Authors: Elham Mansouri, Asghar Mesbahi

Abstract:

Purpose: In the current study, we aimed to investigate the macroscopic and microscopic dose enhancement effect of metallic nanoparticles in interstitial brachytherapy of uterus cancer by Iodin-125 source using a nano-lattice model in MCNPX (5) and MCNP6.1 codes. Materials and methods: Based on a nano-lattice simulation model containing a radiation source and a tumor tissue with cellular compartments loaded with 7mg/g spherical nanoparticles (bismuth, gold, and gadolinium), the energy deposited by the secondary electrons in microscopic and macroscopic level was estimated. Results: The results show that the values of macroscopic DEF is higher than microscopic DEF values and the macroscopic DEF values decreases as a function of distance from the brachytherapy source surface. Also, the results revealed a remarkable discrepancy between the DEF and secondary electron spectra calculated by MCNPX (5) and MCNP6.1 codes, which could be justified by the difference in energy cut-off and electron transport algorithms of two codes. Conclusion: According to the both MCNPX (5) and MCNP6.1 outputs, it could be concluded that the presence of metallic nanoparticles in the tumor tissue of uteruscancer increases the physical effectiveness of brachytherapy by I-125 source. The results presented herein give a physical view of radiosensitization potential of different metallic nanoparticles and could be considered in design of analytical and experimental radiosensitization studies in tumor regions using various radiotherapy modalities in the presence of heavy nanomaterials.

Keywords: MCNPX, MCNP6, nanoparticle, brachytherapy

Procedia PDF Downloads 103
1381 Optimization of Adsorptive Removal of Common Used Pesticides Water Wastewater Using Golden Activated Charcoal

Authors: Saad Mohamed Elsaid, Nabil Anwar, Mahmoud Rushdi

Abstract:

One of the reasons for the intensive use of pesticides is to protect agricultural crops and orchards from pests or agricultural worms. The period of time that pesticides stay inside the soil is estimated at about (2) to (12) weeks. Perhaps the most important reason that led to groundwater pollution is the easy leakage of these harmful pesticides from the soil into the aquifers. This research aims to find the best ways to use traded activated charcoal with gold nitrate solution; for removing the deadly pesticides from the aqueous solution by adsorption phenomenon. The most used pesticides in Egypt were selected, such as Malathion, Methomyl Abamectin and, Thiamethoxam. Activated charcoal doped with gold ions was prepared by applying chemical and thermal treatments to activated charcoal using gold nitrate solution. Adsorption of studied pesticide onto activated carbon /Au was mainly by chemical adsorption, forming a complex with the gold metal immobilized on activated carbon surfaces. In addition, the gold atom was considered as a catalyst to cracking the pesticide molecule. Gold activated charcoal is a low cost material due to the use of very low concentrations of gold nitrate solution. its notice the great ability of activated charcoal in removing selected pesticides due to the presence of the positive charge of the gold ion, in addition to other active groups such as functional oxygen and lignin cellulose. The presence of pores of different sizes on the surface of activated charcoal is the driving force for the good adsorption efficiency for the removal of the pesticides under study The surface area of the prepared char as well as the active groups, were determined using infrared spectroscopy and scanning electron microscopy. Some factors affecting the ability of activated charcoal were applied in order to reach the highest adsorption capacity of activated charcoal, such as the weight of the charcoal, the concentration of the pesticide solution, the time of the experiment, and the pH. Experiments showed that the maximum limit revealed by the batch adsorption study for the adsorption of selected insecticides was in contact time (80) minutes at pH (7.70). These promising results were confirmed, and by establishing the practical application of the developed system, the effect of various operating factors with equilibrium, kinetic and thermodynamic studies is evident, using the Langmuir application on the effectiveness of the absorbent material with absorption capacities higher than most other adsorbents.

Keywords: waste water, pesticides pollution, adsorption, activated carbon

Procedia PDF Downloads 73
1380 Functionalized Spherical Aluminosilicates in Biomedically Grade Composites

Authors: Damian Stanislaw Nakonieczny, Grazyna Simha Martynkova, Marianna Hundakova, G. Kratosová, Karla Cech Barabaszova

Abstract:

The main aim of the research was to functionalize the surface of spherical aluminum silicates in the form of so-called cenospheres. Cenospheres are light ceramic particles with a density between 0.45 and 0.85 kgm-3 hat can be obtained as a result of separation from fly ash from coal combustion. However, their occurrence is limited to about 1% by weight of dry ash mainly derived from anthracite. Hence they are very rare and desirable material. Cenospheres are characterized by complete chemical inertness. Mohs hardness in range of 6 and completely smooth surface. Main idea was to prepare the surface by chemical etching, among others hydrofluoric acid (HF) and hydrogen peroxide, caro acid, silanization using (3-aminopropyl) triethoxysilane (APTES) and tetraethyl orthosilicate (TEOS) to obtain the maximum development and functionalization of the surface to improve chemical and mechanical connection with biomedically used polymers, i.e., polyacrylic methacrylate (PMMA) and polyetheretherketone (PEEK). These polymers are used medically mainly as a material for fixed and removable dental prostheses and PEEK spinal implants. The problem with their use is the decrease in mechanical properties over time and bacterial infections fungal during implantation and use of dentures. Hence, the use of a ceramic filler that will significantly improve the mechanical properties, improve the fluidity of the polymer during shape formation, and in the future, will be able to support bacteriostatic substances such as silver and zinc ions seem promising. In order to evaluate our laboratory work, several instrumental studies were performed: chemical composition and morphology with scanning electron microscopy with Energy-Dispersive X-Ray Probe (SEM/EDX), determination of characteristic functional groups of Fourier Transform Infrared Spectroscopy (FTIR), phase composition of X-ray Diffraction (XRD) and thermal analysis of Thermo Gravimetric Analysis/differentia thermal analysis (TGA/DTA), as well as assessment of isotherm of adsorption with Brunauer-Emmett-Teller (BET) surface development. The surface was evaluated for the future application of additional bacteria and static fungus layers. Based on the experimental work, it was found that orated methods can be suitable for the functionalization of the surface of cenosphere ceramics, and in the future it can be suitable as a bacteriostatic filler for biomedical polymers, i.e., PEEK or PMMA.

Keywords: bioceramics, composites, functionalization, surface development

Procedia PDF Downloads 120
1379 Antibacterial Effect of Silver Diamine Fluoride Incorporated in Fissure Sealants

Authors: Nélio Veiga, Paula Ferreira, Tiago Correia, Maria J. Correia, Carlos Pereira, Odete Amaral, Ilídio J. Correia

Abstract:

Introduction: The application of fissure sealants is considered to be an important primary prevention method used in dental medicine. However, the formation of microleakage gaps between tooth enamel and the fissure sealant applied is one of the most common reasons of dental caries development in teeth with fissure sealants. The association between various dental biomaterials may limit the major disadvantages and limitations of biomaterials functioning in a complementary manner. The present study consists in the incorporation of a cariostatic agent – silver diamine fluoride (SDF) – in a resin-based fissure sealant followed by the study of release kinetics by spectrophotometry analysis of the association between both biomaterials and assessment of the inhibitory effect on the growth of the reference bacterial strain Streptococcus mutans (S. mutans) in an in vitro study. Materials and Methods: An experimental in vitro study was designed consisting in the entrapment of SDF (Cariestop® 12% and 30%) into a commercially available fissure sealant (Fissurit®), by photopolymerization and photocrosslinking. The same sealant, without SDF was used as a negative control. The effect of the sealants on the growth of S. mutans was determined by the presence of bacterial inhibitory halos in the cultures at the end of the incubation period. In order to confirm the absence of bacteria in the surface of the materials, Scanning Electron Microscopy (SEM) characterization was performed. Also, to analyze the release profile of SDF along time, spectrophotometry technique was applied. Results: The obtained results indicate that the association of SDF to a resin-based fissure sealant may be able to increase the inhibition of S. mutans growth. However, no SDF release was noticed during the in vitro release studies and no statistical significant difference was verified when comparing the inhibitory halo sizes obtained for test and control group.  Conclusions: In this study, the entrapment of SDF in the resin-based fissure sealant did not potentiate the antibacterial effect of the fissure sealant or avoid the immediate development of dental caries. The development of more laboratorial research and, afterwards, long-term clinical data are necessary in order to verify if this association between these biomaterials is effective and can be considered for being used in oral health management. Also, other methodologies for associating cariostatic agents and sealant should be addressed.

Keywords: biomaterial, fissure sealant, primary prevention, silver diamine fluoride

Procedia PDF Downloads 259
1378 Sample Preparation and Coring of Highly Friable and Heterogeneous Bonded Geomaterials

Authors: Mohammad Khoshini, Arman Khoshghalb, Meghdad Payan, Nasser Khalili

Abstract:

Most of the Earth’s crust surface rocks are technically categorized as weak rocks or weakly bonded geomaterials. Deeply weathered, weakly cemented, friable and easily erodible, they demonstrate complex material behaviour and understanding the overlooked mechanical behaviour of such materials is of particular importance in geotechnical engineering practice. Weakly bonded geomaterials are so susceptible to surface shear and moisture that conventional methods of core drilling fail to extract high-quality undisturbed samples out of them. Moreover, most of these geomaterials are of high heterogeneity rendering less reliable and feasible material characterization. In order to compensate for the unpredictability of the material response, either numerous experiments are needed to be conducted or large factors of safety must be implemented in the design process. However, none of these approaches is sustainable. In this study, a method for dry core drilling of such materials is introduced to take high-quality undisturbed core samples. By freezing the material at certain moisture content, a secondary structure is developed throughout the material which helps the whole structure to remain intact during the core drilling process. Moreover, to address the heterogeneity issue, the natural material was reconstructed artificially to obtain a homogeneous material with very high similarity to the natural one in both micro and macro-mechanical perspectives. The method is verified for both micro and macro scale. In terms of micro-scale analysis, using Scanning Electron Microscopy (SEM), pore spaces and inter-particle bonds were investigated and compared between natural and artificial materials. X-Ray Diffraction, XRD, analyses are also performed to control the chemical composition. At the macro scale, several uniaxial compressive strength tests, as well as triaxial tests, were performed to verify the similar mechanical response of the materials. A high level of agreement is observed between micro and macro results of natural and artificially bonded geomaterials. The proposed methods can play an important role to cut down the costs of experimental programs for material characterization and also to promote the accuracy of the numerical modellings based on the experimental results.

Keywords: Artificial geomaterial, core drilling, macro-mechanical behavior, micro-scale, sample preparation, SEM photography, weakly bonded geomaterials

Procedia PDF Downloads 216
1377 Factors Controlling Marine Shale Porosity: A Case Study between Lower Cambrian and Lower Silurian of Upper Yangtze Area, South China

Authors: Xin Li, Zhenxue Jiang, Zhuo Li

Abstract:

Generally, shale gas is trapped within shale systems with low porosity and ultralow permeability as free and adsorbing states. Its production is controlled by properties, in terms of occurrence phases, gas contents, and percolation characteristics. These properties are all influenced by porous features. In this paper, porosity differences of marine shales were explored between Lower Cambrian shale and Lower Silurian shale of Sichuan Basin, South China. Both the two shales were marine shales with abundant oil-prone kerogen and rich siliceous minerals. Whereas Lower Cambrian shale (3.56% Ro) possessed a higher thermal degree than that of Lower Silurian shale (2.31% Ro). Samples were measured by a combination of organic-chemistry geology measurement, organic matter (OM) isolation, X-ray diffraction (XRD), N2 adsorption, and focused ion beam milling and scanning electron microscopy (FIB-SEM). Lower Cambrian shale presented relatively low pore properties, with averaging 0.008ml/g pore volume (PV), averaging 7.99m²/g pore surface area (PSA) and averaging 5.94nm average pore diameter (APD). Lower Silurian shale showed as relatively high pore properties, with averaging 0.015ml/g PV, averaging 10.53m²/g PSA and averaging 18.60nm APD. Additionally, fractal analysis indicated that the two shales presented discrepant pore morphologies, mainly caused by differences in the combination of pore types between the two shales. More specifically, OM-hosted pores with pin-hole shape and dissolved pores with dead-end openings were the main types in Lower Cambrian shale, while OM-hosted pore with a cellular structure was the main type in Lower Silurian shale. Moreover, porous characteristics of isolated OM suggested that OM of Lower Silurian shale was more capable than that of Lower Cambrian shale in the aspect of pore contribution. PV of isolated OM in Lower Silurian shale was almost 6.6 times higher than that in Lower Cambrian shale, and PSA of isolated OM in Lower Silurian shale was almost 4.3 times higher than that in Lower Cambrian shale. However, no apparent differences existed among samples with various matrix compositions. At late diagenetic or metamorphic epoch, extensive diagenesis overprints the effects of minerals on pore properties and OM plays the dominant role in pore developments. Hence, differences of porous features between the two marine shales highlight the effect of diagenetic degree on OM-hosted pore development. Consequently, distinctive pore characteristics may be caused by the different degrees of diagenetic evolution, even with similar matrix basics.

Keywords: marine shale, lower Cambrian, lower Silurian, om isolation, pore properties, om-hosted pore

Procedia PDF Downloads 134
1376 Fabrication and Mechanical Characterization of Sugarcane Bagasse Fiber-Reinforced Polypropylene Based Composites: Effect of Gamma Radiation

Authors: Kamrun N. Keya, Nasrin A. Kona, Ruhul A. Khan

Abstract:

Sugarcane bagasse (SCB)-reinforced Polypropylene (PP) Based matrix composites (25-45 wt% fiber) were fabricated by a compression molding technique. The SCB surface was chemically modified using 5%-10% sodium hydroxide (NaOH), and after that, mechanical properties, water uptake, and soil degradation of the composites were investigated. Tensile strength (TS), tensile modulus (TM), bending strength (BS), bending modulus (BM) and elongation at break (Eb%) of the 30wt% composites were found to be 35.6 MPa, 10.2 GPa, 56 MPa, 5.6 GPa, and 11%, respectively. The SCB/PP based composites were treated with irradiated under gamma radiation (the source strength 50 kCi Cobalt-60) of various doses (2.5 kGy to 10 kGy). The effect of gamma radiation on the composites was also investigated, and it found that the effect of 5.0 kGy (i.e. units for radiation measurement is 'gray', kGy=kilogray ) gamma dose showed better mechanical properties than other doses. The results revealed that the combination of the chemical modification of the SCB fibers and irradiation of the composites were more effective in compatibility improvement than chemical modification alone. After flexural testing, fracture sides of the untreated and treated both composites were studied by scanning electron microscope (SEM). SEM results of the treated SCB/PP based composites showed better fiber-matrix adhesion than untreated SCB/PP based composites. However, it was found that the treated SCB/PP composite has better mechanical strength, durability, and more receptivity than untreated SCB/PP based composite.

Keywords: sugarcane bagasse (SCB), polypropylene (PP), mechanical properties, scanning electron microscope (SEM), gamma radiation, water uptake tests and soil degradation

Procedia PDF Downloads 138
1375 Suture Biomaterials Development from Natural Fibers: Muga Silk (Antheraea assama) and Ramie (Boehmeria nivea)

Authors: Raghuram Kandimalla, Sanjeeb Kalita, Bhaswati Choudhury, Jibon Kotoky

Abstract:

The quest for developing an ideal suture material prompted our interest to develop a novel suture with advantageous characteristics to market available ones. We developed novel suture biomaterial from muga silk (Antheraea assama) and ramie (Boehmeria nivea) plant fiber. Field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), attenuated total reflection fourier transform infrared spectroscopy (ATR-FTIR) and thermo gravimetric analysis (TGA) results revealed the physicochemical properties of the fibers which supports the suitability of fibers for suture fabrication. Tensile properties of the prepared sutures were comparable with market available sutures and it found to be biocompatible towards human erythrocytes and nontoxic to mammalian cells. The prepared sutures completely healed the superficial deep wound incisions within seven days in adult male wister rats leaving no rash and scar. Histopathology studies supports the wound healing ability of sutures, as rapid synthesis of collagen, connective tissue and other skin adnexal structures were observed within seven days of surgery. Further muga suture surface modified by exposing the suture to oxygen plasma which resulted in formation of nanotopography on suture surface. Broad spectrum antibiotic amoxicillin was functionalized on the suture surface to prepare an advanced antimicrobial muga suture. Surface hydrophilicity induced by oxygen plasma results in an increase in drug-impregnation efficiency of modified muga suture by 16.7%. In vitro drug release profiles showed continuous and prolonged release of amoxicillin from suture up to 336 hours. The advanced muga suture proves to be effective against growth inhibition of Staphylococcus aureus and Escherichia coli, whereas normal muga suture offers no antibacterial activity against both types of bacteria. In vivo histopathology studies and colony-forming unit count data revealed accelerated wound healing activity of advanced suture over normal one through rapid synthesis and proliferation of collagen, hair follicle and connective tissues.

Keywords: sutures, biomaterials, silk, Ramie

Procedia PDF Downloads 317
1374 Characterizing Surface Machining-Induced Local Deformation Using Electron Backscatter Diffraction

Authors: Wenqian Zhang, Xuelin Wang, Yujin Hu, Siyang Wang

Abstract:

The subsurface layer of a component plays a significant role in its service performance. Any surface mechanical process during fabrication can introduce a deformed layer near the surface, which can be related to the microstructure alteration and strain hardening, and affects the mechanical properties and corrosion resistance of the material. However, there exists a great difficulty in determining the subsurface deformation induced by surface machining. In this study, electron backscatter diffraction (EBSD) was used to study the deformed layer of surface milled 316 stainless steel. The microstructure change was displayed by the EBSD maps and characterized by misorientation variation. The results revealed that the surface milling resulted in heavily nonuniform deformations in the subsurface layer and even in individual grains. The direction of the predominant grain deformation was about 30-60 deg to the machined surface. Moreover, a local deformation rate (LDR) was proposed to quantitatively evaluate the local deformation degree. Both of the average and maximum LDRs were utilized to characterize the deformation trend along the depth direction. It was revealed that the LDR had a strong correlation with the development of grain and sub-grain boundaries. In this work, a scan step size of 1.2 μm was chosen for the EBSD measurement. A LDR higher than 18 deg/μm indicated a newly developed grain boundary, while a LDR ranged from 2.4 to 18 deg/μm implied the generation of a sub-grain boundary. And a lower LDR than 2.4 deg/μm could only introduce a slighter deformation and no sub-grain boundary was produced. According to the LDR analysis with the evolution of grain or sub grain boundaries, the deformed layer could be classified into four zones: grain broken layer, seriously deformed layer, slightly deformed layer and non-deformed layer.

Keywords: surface machining, EBSD, subsurface layer, local deformation

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