Search results for: dielectric spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 2306

Search results for: dielectric spectroscopy

716 Development of Mg-Containing Hydroxyapatite-Based Bioceramics From Phosphate Rock for Bone Applications

Authors: Sara Mercedes Barroso Pinzón, Álvaro Jesús Caicedo Castro, Antonio Javer Sánchez Herencia

Abstract:

In recent years there has been increased academic and industrial research into the development of orthopaedic implants with structural properties and functionality similar to mechanical strength, osseointegration, thermal stability and antibacterial capacity similar to bone structure. Hydroxyapatite has been considered for decades as an ideal biomaterial for bone regeneration due to its chemical and crystallographic similarity to the mineral structure bioapatites. However, the lack of trace elements in the hydroxyapatite structure confers very low mechanical and biological properties. Under this scenario, the objective of the research is the synthesis of hydroxyapatite with Mg from the francolite mineral present in phosphate rock from the central-eastern region of Colombia, taking advantage of the extraction of mineral species as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with magnesium carbonates and quartz. The chemical and mineralogical composition was determined by X-ray fluorescence (XRF) and X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX); the optimum conditions were established using the acid leaching mechanism in the wet concentration process. From the products obtained and characterised by XRD, XRF, SEM, FTIR, RAMAN, HAp-Mg biocomposite scaffolds are fabricated and the influence of Mg on morphometric parameters, mechanical and biological properties in the formed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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715 Fluoride Removal from Groundwater in the East Nile Area (Sudan) Using Locally Available Charcoal

Authors: Motwkel M. Alhaj, Bashir M. Elhassan

Abstract:

The East Nile area is located in Khartoum state. The main source of drinking water in the East Nile Area (Sudan) is groundwater. However, fluoride concentration in the water is more than the maximum allowable dose, which is 1.5 mg/l. This study aims to demonstrate and innovative, affordable, and efficient filter to remove fluoride from drinking water. Many researchers have found that aluminum oxide-coated adsorbent is the most affordable technology for fluoride removal. However, adsorption is pH-dependent, and the water pH in the East Nile area is relatively high (around 8), which is hindering the adsorption process. Locally available charcoal was crushed, sieved, and coated with aluminum oxide. Then, different coating configurations were tested in order to produce an adsorbent with a high pH point of zero charge pH PZC in order to overcome the effect of high pH of water. Moreover, different methods were used to characterize the adsorbent, including: Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Spectroscopy (EDX), Brunauer - Emmett - Teller (BET) method, and pH point of zero charge pH PZC. The produced adsorbent has pH PZC of 8.5, which is essential in enhancing the fluoride adsorption process. A pilot household fluoride filter was also designed and installed in a house that has water with 4.34 mg/l F- and pH of 8.4. The filter was operated at a flow rate 250 cm³/min. The total cost of treating one cubic meter was about 0.63$, while the cost for the same water before adsorbent coating modification was 2.33$⁄cm³.

Keywords: water treatment, fluoride, adsorption, charcoal, Sudan

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714 Layer by Layer Coating of Zinc Oxide/Metal Organic Framework Nanocomposite on Ceramic Support for Solvent/Solvent Separation Using Pervaporation Method

Authors: S. A. A. Nabeela Nasreen, S. Sundarrajan, S. A. Syed Nizar, Seeram Ramakrishna

Abstract:

Metal-organic frameworks (MOFs) have attracted considerable interest due to its diverse pore size tunability, fascinating topologies and extensive uses in fields such as catalysis, membrane separation, chemical sensing, etc. Zeolitic imidazolate frameworks (ZIFs) are a class of MOF with porous crystals containing extended three-dimensional structures of tetrahedral metal ions (e.g., Zn) bridged by Imidazolate (Im). Selected ZIFs are used to separate solvent/solvent mixtures. A layer by layer formation of the nanocomposite of Zinc oxide (ZnO) and ZIF on a ceramic support using a solvothermal method was engaged and tested for target solvent/solvent separation. Metal oxide layer was characterized by XRD, SEM, and TEM to confirm the smooth and continuous coating for the separation process. The chemical composition of ZIF films was studied by using X-Ray absorption near-edge structure (XANES) spectroscopy. The obtained ceramic tube with metal oxide and ZIF layer coating were tested for its packing density, thickness, distribution of seed layers and variation of permeation rate of solvent mixture (isopropyl alcohol (IPA)/methyl isobutyl ketone (MIBK). Pervaporation technique was used for the separation to achieve a high permeation rate with separation ratio of > 99.5% of the solvent mixture.

Keywords: metal oxide, membrane, pervaporation, solvothermal, ZIF

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713 Potential Use of Local Materials as Synthesizing One Part Geopolymer Cement

Authors: Areej Almalkawi, Sameer Hamadna, Parviz Soroushian, Nalin Darsana

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The work on indigenous binders in this paper focused on the following indigenous raw materials: red clay, red lava and pumice (as primary aluminosilicate precursors), wood ash and gypsum (as supplementary minerals), and sodium sulfate and lime (as alkali activators). The experimental methods used for evaluation of these indigenous raw materials included laser granulometry, x-ray fluorescence (XRF) spectroscopy, and chemical reactivity. Formulations were devised for transforming these raw materials into alkali aluminosilicate-based hydraulic cements. These formulations were processed into hydraulic cements via simple heating and milling actions to render thermal activation, mechanochemical and size reduction effects. The resulting hydraulic cements were subjected to laser granulometry, heat of hydration and reactivity tests. These cements were also used to prepare mortar mixtures, which were evaluated via performance of compressive strength tests. The measured values of strength were correlated with the reactivity, size distribution and microstructural features of raw materials. Some of the indigenous hydraulic cements produced in this reporting period yielded viable levels of compressive strength. The correlation trends established in this work are being evaluated for development of simple and thorough methods of qualifying indigenous raw materials for use in production of indigenous hydraulic cements.

Keywords: one-part geopolymer cement, aluminosilicate precursors, thermal activation, mechanochemical

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712 Fabrication and Characterization of PPy/rGO|PPy/ZnO Composite with Varying Zno Concentration as Anode for Fuel Cell Applications

Authors: Bryan D. Llenarizas, Maria Carla F. Manzano

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The rapid growth of electricity demand has led to a pursuit of alternative energy sources with high power output and not harmful to the environment. The fuel cell is a device that generates electricity via chemical reactions between the fuel and oxidant. Fuel cells have been known for decades, but the development of high-power output and durability was still one of the drawbacks of this energy source. This study investigates the potential of layer-by-layer composite for fuel cell applications. A two-electrode electrochemical cell was used for the galvanostatic electrochemical deposition method to fabricate a Polypyrrole/rGO|Polypyrrole/ZnO layer-by-layer composite material for fuel cell applications. In the synthesis, the first layer comprised 0.1M pyrrole monomer and 1mg of rGO, while the second layer had 0.1M pyrrole monomer and variations of ZnO concentration ranging from 0.08M up to 0.12M. A constant current density of 8mA/cm² was applied for 1 hour in fabricating each layer. Scanning electron microscopy (SEM) for the fabricated LBL material shows a globular surface with white spots. These white spots are the ZnO particles confirmed by energy-dispersive X-ray spectroscopy, indicating a successful deposition of the second layer onto the first layer. The observed surface morphology was consistent for each variation of ZnO concentrations. AC measurements were conducted to obtain the AC resistance of the fabricated film. Results show a decrease in AC resistance as the concentration of ZnO increases.

Keywords: anode, composite material, electropolymerization, fuel cell, galvanostatic, polypyrrole

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711 Development of Lectin-Based Biosensor for Glycoprofiling of Clinical Samples: Focus on Prostate Cancer

Authors: Dominika Pihikova, Stefan Belicky, Tomas Bertok, Roman Sokol, Petra Kubanikova, Jan Tkac

Abstract:

Since aberrant glycosylation is frequently accompanied by both physiological and pathological processes in a human body (cancer, AIDS, inflammatory diseases, etc.), the analysis of tumor-associated glycan patterns have a great potential for the development of novel diagnostic approaches. Moreover, altered glycoforms may assist as a suitable tool for the specificity and sensitivity enhancement in early-stage prostate cancer diagnosis. In this paper we discuss the construction and optimization of ultrasensitive sandwich biosensor platform employing lectin as glycan-binding protein. We focus on the immunoassay development, reduction of non-specific interactions and final glycoprofiling of human serum samples including both prostate cancer (PCa) patients and healthy controls. The fabricated biosensor was measured by label-free electrochemical impedance spectroscopy (EIS) with further lectin microarray verification. Furthermore, we analyzed different biosensor interfaces with atomic force microscopy (AFM) in nanomechanical mapping mode showing a significant differences in the altitude. These preliminary results revealing an elevated content of α-2,3 linked sialic acid in PCa patients comparing with healthy controls. All these experiments are important step towards development of point-of-care devices and discovery of novel glyco-biomarkers applicable in cancer diagnosis.

Keywords: biosensor, glycan, lectin, prostate cancer

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710 In vitro Disaggregation and Dissolution of Four IR Lamotrigine Solid Dosage Forms

Authors: Ilaria Manca, Ilaria Manca, Francesca Pettinau, Ignazia Mocci, Elisabetta M. Usai, Barbara Pittau

Abstract:

Lamotrigine is a phenyltriazine used in the treatment of epilepsy and bipolar disorder type I. The purpose of this study was to test and compare various solid forms of immediate release (IR) lamotrigine products, at different strenghts, in order to study their disaggregation and dissolution behavior. IR products are designed to release their active substance promptly after administration. Concentration of hydrochloric acid in gastric juice is about 0.1-0.001 M, so FDA (Food and Drug Administration) recommends, for lamotrigine regular tablets, dissolution tests in HCl 0.1 M.Toinvestigate the pH dependency of drug release in the entire gastrointestinal tract, we worked at two additional media with different pH values (4.5 and 6.8), that reflect conditions in it. To afford acceptable dissolution rates, tablets must disintegrate. Disaggregation of constituent particles increases the surface area and substantially increases the dissolution rate. For this reason availability of an active substance from tablets depends on its ability to disintegrate fast in dissolution media. pH of gastrointestinal fluid affects drug absorption by conditioning its solubility and dissolution, but also tablet disintegration may be influenced by it. To obtain information about the quantitative relationship between different mixture components, Nuclear Magnetic Resonance (NMR) spectroscopy was used. We also investigate tablet hardness. The investigation carried out confirms pH 1.2 as the ideal environment for the immediate availability of the active substance.

Keywords: dissolution, disaggregation, Lamotrigine, bioequivalence

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709 Effect of the Nature of Silica Precursor in Zeolite ZSM-22 Synthesis

Authors: Nyiko M. Chauke, James Ramontja, Richard M. Moutloali

Abstract:

The zeolite ZSM-22 material demonstrated effective hydrophilic character as a nanoadditive filler in the preparation of nanocomposite membranes. In this study, nanorods ZSM-22 zeolite materials were hydrothermally synthesised from a homogenous gel mixture prepared using different silica precursors: colloidal silica, fumed silica, tetraethylorthosilicate (TEOS), and aluminium precursor: aluminium sulphate octadecahydrate (Al₂(SO₄)₃.18H₂O to Si/Al of 60. This was focused on developing a defect-free zeolite framework for effective use in applications such as membrane separation process, adsorption, and catalysis. The obtained ZSM-22 zeolite materials with 60 Si/Al ratio exhibits high crystallinity, hydrophilicity, and needle-like morphologies, suggesting successful synthesis as shown by X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Fourier-Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) physicochemical analysis. It was revealed that the use of different nature of silica precursors significantly influenced the properties of the final product and contributed to the development of defect-free zeolite material. As such, the crystalline nanorods of Theta-1 (TON) ZSM-22 obtained from TEOS silica showed high phase purity, defect-free, and narrow particle size distribution. Morphological analysis exhibited that the use of TEOS as silica precursor was effective than its counterparts and produced high crystalline need-like agglomerated particles.

Keywords: silica precursor, hydrothermal synthesis, zeolite material, ZSM-22

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708 GIS-Based Spatial Distribution and Evaluation of Selected Heavy Metals Contamination in Topsoil around Ecton Mining Area, Derbyshire, UK

Authors: Zahid O. Alibrahim, Craig D. Williams, Clive L. Roberts

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The study area (Ecton mining area) is located in the southern part of the Peak District in Derbyshire, England. It is bounded by the River Manifold from the west. This area has been mined for a long period. As a result, huge amounts of potentially toxic metals were released into the surrounding area and are most likely to be a significant source of heavy metal contamination to the local soil, water and vegetation. In order to appraise the potential heavy metal pollution in this area, 37 topsoil samples (5-20 cm depth) were collected and analysed for their total content of Cu, Pb, Zn, Mn, Cr, Ni and V using ICP (Inductively Coupled Plasma) optical emission spectroscopy. Multivariate Geospatial analyses using the GIS technique were utilised to draw geochemical maps of the metals of interest over the study area. A few hotspot points, areas of elevated concentrations of metals, were specified, which are presumed to be the results of anthropogenic activities. In addition, the soil’s environmental quality was evaluated by calculating the Mullers’ Geoaccumulation index (I geo), which suggests that the degree of contamination of the investigated heavy metals has the following trend: Pb > Zn > Cu > Mn > Ni = Cr = V. Furthermore, the potential ecological risk, using the enrichment factor (EF), was also specified. On the basis of the calculated amount or the EF, the levels of pollution for the studied metals in the study area have the following order: Pb>Zn>Cu>Cr>V>Ni>Mn.

Keywords: enrichment factor, geoaccumulation index, GIS, heavy metals, multivariate analysis

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707 Effects of Gelatin on Characteristics and Dental Pathogen Inhibition by Silver Nanoparticles Synthesized from Ascorbic Acid

Authors: Siriporn Okonogi, Temsiri Suwan, Sakornrat Khongkhunthian, Jakkapan Sirithunyalug

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In this study, silver nanoparticles (AgNPs) were prepared using ascorbic acid as a reducing agent and silver nitrate as a precursor. The effects of gelatin (G) on particle characteristics and dental pathogen inhibition were investigated. The spectra of AgNPs and G-AgNPs were compared using UV-Vis and Energy-dispersive X-ray (EDX) spectroscopy. The obtained AgNPs and G-AgNPs showed the maximum absorption at 410 and 430 nm, respectively, and EDX spectra of both systems confirmed Ag element. Scanning electron microscope showed that AgNPs and G-AgNPs were spherical in shape. Particles size, size distribution, and zeta potential were determined using dynamic light scattering approach. The size of AgNPs and G-AgNPs were 56 ± 2.4 and 67 ± 3.6 nm, respectively with a size distribution of 0.23 ± 0.03 and 0.19 ± 0.02, respectively. AgNPs and G-AgNPs exhibited negative zeta potential of 24.1 ± 2.7 mV and 32.7 ± 1.2 mV, respectively. Minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of the obtained AgNPs and G-AgNPs against three strains of dental pathogenic bacteria; Streptococcus gordonii, Streptococcus mutans, and Staphylococcus aureus were determined using broth dilution method. AgNPs and G-AgNPs showed the strongest inhibition against S. gordonii with the MIC of 0.05 and 0.025 mg/mL, respectively and the MBC of 0.1 and 0.05 mg/mL, respectively. Cytotoxicity test of AgNPs and G-AgNPs on human breast cancer cells using MTT assay indicated that G-AgNPs (0.1 mg/mL) was significantly stronger toxic than AgNPs with the cell inhibition of 91.1 ± 5.4%. G-AgNPs showed significantly less aggregation after storage at room temperature for 90 days than G-AgNPs.

Keywords: antipathogenic activity, ascorbic acid, cytotoxicity, stability

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706 Shape Evolution of CdSe Quantum Dots during the Synthesis in the Presence of Silver Halides

Authors: Pavel Kotin, Sergey Dotofeev, Daniil Kozlov, Alexey Garshev

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We propose the investigation of CdSe quantum dots which were synthesized in the presence of silver halides. To understand a process of nanoparticle formation in more detail, we varied the silver halide amount in the synthesis and proposed a sampling during colloidal growth. The attempts were focused on the investigation of shape, structure and optical properties of nanoparticles. We used the colloidal method of synthesis. Cadmium oleate, tri-n-octylphosphine selenide (TOPSe) and AgHal in TOP were precursors of cadmium, selenium and silver halides correspondingly. The molar Ag/Cd ratio in synthesis was varied from 1/16 to 1/1. The sampling was basically realized in 20 sec, 5 min, and 30 min after the beginning of quantum dots nucleation. To investigate nanoparticles we used transmission electron microscopy (including high resolution one), X-ray diffraction, and optical spectroscopy. It was established that silver halides lead to obtaining tetrapods with different leg length and large ellipsoidal nanoparticles possessing an intensive near IR photoluminescence. The change of the amount of silver halide in synthesis and the selection of an optimal growth time allows controlling the shape and the share of tetrapods or ellipsoidal nanoparticles in the product. Our main attempts were focused on a detailed investigation of the quantum dots structure and shape evolution and, finally, on mechanisms of such nanoparticle formation.

Keywords: colloidal quantum dots, shape evolution, silver doping, tetrapods

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705 Growth Model and Properties of a 3D Carbon Aerogel

Authors: J. Marx, D. Smazna, R. Adelung, B. Fiedler

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Aerographite is a 3D interconnected carbon foam. Its tetrapodal morphology is based on the zinc oxide (ZnO) template structure, which is replicated in the chemical vapour deposition (CVD) into a hollow carbon structure. This replication process is analyzed in ex-situ studies via interrupted synthesis and the observation of the reaction progress by using scanning electron (SEM), transmission electron microscopy (TEM) and Raman spectroscopy techniques. Based on the epitaxial growth process, with a layer-by-layer growth behaviour of the wall thickness or number of layers and the catalytical graphitization of the deposited amorphous carbon into graphitic carbon by zinc, a growth model is created. The properties of aerographite, such as the electrical conductivity is dependent on the graphitization and number of layer (wall thickness). Wall thicknesses between 3 nm and 22 nm are achieved by a controlled stepwise reduction of the synthesis time on the basis of the developed growth model, and by a further thermal treatment at 1800 °C the graphitization of the presented carbon foam is modified. The variation of the wall thickness leads to an optimum defect density (ID/IG ratio) and the graphitization to an improvement in the electrical conductivity. Furthermore, a metallic conducting behaviour of untreated and 1800 °C treated aerographite can be observed. Due to these structural and defective modifications, a fundamental structural-property equation for the description of their influences on the electrical conductivity is developed.

Keywords: electrical conductivity, electron microscopy (SEM/TEM), graphitization, wall thickness

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704 Experimental and Numerical Determination of the Freeze Point Depression of a Multi-Phase Flow in a Scraped Surface Heat Exchanger

Authors: Carlos A. Acosta, Amar Bhalla, Ruyan Guo

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Scraped surface heat exchangers (SSHE) use a rotor shaft assembly with scraping blades to homogenize viscous fluids during the heat transfer process. Obtaining in-situ measurements is difficult because the rotor and scraping blades spin continuously inside the mixing chamber, obstructing the instrumentation pathway. Computational fluid dynamics simulations provide useful insight into the flow behavior around the scraper blades for a variety of fluids and blade geometries. However, numerical solutions often focus on the fluid dynamics and heat transfer phenomena of rotating flow, ignoring the glass-transition temperature and freezing point depression. This research studies the multi-phase fluid dynamics and freezing point depression inside the SSHE with non-isothermal conditions in a time dependent process using an aqueous solution that contains 13.5 wt.% high fructose corn syrup and CO₂. The computational results were validated with in-situ pressure, temperature, and optical spectroscopy measurements. Results from the numerical model show good quantitatively agreement with experimental values.

Keywords: computational fluid dynamics, freezing point depression, phase-transition temperature, multi-phase flow

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703 Evaluation of ROS Mediated Apoptosis Induced by Tuber Extract of Dioscorea Bulbifera on Human Breast Adenocarcinoma

Authors: Debasmita Dubey, Rajesh Kumar Meher, Smruti Pragya Samal, Pradeep Kumar Naik

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Background: To determine antioxidant properties and anticancer activity by ROS and mitochondrial transmembrane potential mediated apoptosis against MCF7, MDA-MB-231, cell line. Methods: Leaf sample was extracted using methanol by microwave digestion technique. The antioxidant properties of the methanolic extract were determined by a DPPH scavenging assay. In vitro anticancer activity, mitochondrial transmembrane potential, apoptosis activity and DNA fragmentation study, as well as intracellular ROS activity of most potential leaf extract, were also determined by using the MDA-MB-231cell line. In vivo animal toxicity study was carried out using mice model. Results: Methanolic leaf extract has shown the highest antioxidant, as well as anticancer activity, is based on the assay conducted. For the identification of active phytochemicals from methanolic extract, High-resolution mass spectroscopy-LCMS was used. In vitro cytotoxicity study against MCF-7 and MDA-MB-231 cell line and IC 50 value was found to be 37.5µg/ml. From histopathological studies, no toxicity in liver and kidney tissue was identified. Conclusion: This plant tuber can be used as a regular diet to reduce the chance of breast cancer. Further, more studies should be conducted to isolate and identify the responsible compound.

Keywords: human breast adenocarcinoma, ROS, mitochondrial transmembrane, apoptosis

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702 Bioremoval of Malachite Green Dye from Aqueous Solution Using Marine Algae: Isotherm, Kinetic and Mechanistic Study

Authors: M. Jerold, V. Sivasubramanian

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This study reports the removal of Malachite Green (MG) from simulated wastewater by using marine macro algae Ulva lactuca. Batch biosorption experiments were carried out to determine the biosorption capacity. The biosorption capacity was found to be maximum at pH 10. The effect of various other operation parameters such as biosorbent dosage, initial dye concentration, contact time and agitation was also investigated. The equilibrium attained at 120 min with 0.1 g/L of biosorbent. The isotherm experimental data fitted well with Langmuir Model with R² value of 0.994. The maximum Langmuir biosorption capacity was found to be 76.92 mg/g. Further, Langmuir separation factor RL value was found to be 0.004. Therefore, the adsorption is favorable. The biosorption kinetics of MG was found to follow pseudo second-order kinetic model. The mechanistic study revealed that the biosorption of malachite onto Ulva lactuca was controlled by film diffusion. The solute transfer in a solid-liquid adsorption process is characterized by the film diffusion and/or particle diffusion. Thermodynamic study shows ΔG° is negative indicates the feasibility and spontaneous nature for the biosorption of malachite green. The biosorbent was characterized using Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and elemental analysis (CHNS: Carbon, Hydrogen, Nitrogen, Sulphur). This study showed that Ulva lactuca can be used as promising biosorbent for the removal of MG from wastewater.

Keywords: biosorption, Ulva lactuca, wastewater, malachite green, isotherm, kinetics

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701 Impact of Microwave Heating Temperatures on the Pharmaceutical Powder Characteristics

Authors: Maha Al-Ali, Selvakannan Periasamy, Rajarathinam Parthasarathy

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Drying temperature is an important factor impacting the physicochemical properties of the dried materials, particularly the pharmaceutical powders. Drying of pharmaceuticals by using microwave radiation is very limited, and the available information about the interaction between the electromagnetic radiations and the pharmaceutical material is still scarce. Therefore, microwave drying process is employed in this work to dry the wet (moisturised) granules of the formulated naproxen-sodium drug. This study aims to investigate the influences of the microwave radiation temperatures on the moisture removal, the crystalline structure, the size and morphology of the dried naproxen-sodium particles, and identify any potential changes in the chemical groups of the drug. In this work, newly formulated naproxen-sodium is prepared and moisturized by wet granulation process and hence dried by using microwave radiation at different temperatures. Moisture analyzer, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and scanning electron microscope are used to characterise the non-moisturised powder (reference powder), the moisturised granules, and the dried particles. The results show that microwave drying of naproxen-sodium at high drying temperature is more efficient than that at low temperatures in terms of the moisture removal. Although there is no significant change in the chemical structure of the dried particles, the particle size, crystallinity and morphology are relatively changed with changing of heating temperature.

Keywords: heating temperature, microwave drying, naproxen-sodium, particle size

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700 Bimetallic Silver-Platinum Core-Shell Nanoparticles Formation and Spectroscopic Analysis

Authors: Mangaka C. Matoetoe, Fredrick O. Okumu

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Metal nanoparticles have attracted a great interest in scientific research and industrial applications, owing to their unique large surface area-to-volume ratios and quantum-size effects. Supported metal nanoparticles play a pivotal role in areas such as nanoelectronics, energy storage and as catalysts for the sustainable production of fuels and chemicals. Monometallics (Ag, Pt) and Silver-platinum (Ag-Pt) bimetallic (BM) nanoparticles (NPs) with a mole fraction (1:1) were prepared by reduction / co-reduction of hexachloroplatinate and silver nitrate with sodium citrate. The kinetics of the nanoparticles formation was monitored using UV-visible spectrophotometry. Transmission electron microscopy (TEM) and Energy-dispersive X-ray (EDX) spectroscopy were used for size, film morphology as well as elemental composition study. Fast reduction processes was noted in Ag NPs (0.079 s-1) and Ag-Pt NPs 1:1 (0.082 s-1) with exception of Pt NPs (0.006 s-1) formation. The UV-visible spectra showed characteristic peaks in Ag NPs while the Pt NPs and Ag-Pt NPs 1:1 had no observable absorption peaks. UV visible spectra confirmed chemical reduction resulting to formation of NPs while TEM images depicted core-shell arrangement in the Ag-Pt NPs 1:1 with particle size of 20 nm. Monometallic Ag and Pt NPs reported particle sizes of 60 nm and 2.5 nm respectively. The particle size distribution in the BM NPs was found to directly depend on the concentration of Pt NPs around the Ag core. EDX elemental composition analysis of the nanoparticle suspensions confirmed presence of the Ag and Pt in the Ag-Pt NPs 1:1. All the spectroscopic analysis confirmed the successful formation of the nanoparticles.

Keywords: kinetics, morphology, nanoparticles, platinum, silver

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699 Determination of Heavy Metals in Canned Dry-Milk and Fish from Supermarkets in Addis Ababa

Authors: Kefyalew Muleta, Tetemke Mehari

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Background: Human being require metallic elements such as copper and zinc up to certain limits that could cause problems if found in excess. Other metallic elements like cadmium and lead can be harmful to health if foodstuffs containing them are consumed regularly. Canned dry-milk and fish contain these metals in the journey from farm to fork. Objective: This study was designed to determine the concentration of Cd, Cu, Pb, and Zn in four brands of canned dry-milk and fish from supermarkets in Addis Ababa. Methods: Laboratory based cross-sectional study design was used to determine the concentration of the heavy metals in four different brands of canned dry-milk and fish imported from different country from February to March 2013. The foods brands were sampled by simple random sampling method from eight supermarkets in Addis Ababa and coded. Wet oxidation using HNO3 and H2O2 was used to extract the heavy metals from the foods samples and analyzed by Flame Atomic Absorption Spectroscopy. Conclusions: From this study, it can be concluded that the level of Cadmium and Copper residues in canned dry-milk significantly vary among brands; and the levels of copper residue significantly vary among brands of canned fish at 95 % level. The AM milk brand from Ethiopia was safe in cadmium level. The cadmium and lead level in the NF fish brands from Indonesia packed in vegetables oil, and the lead level in DF brand packed in brine are safe.

Keywords: AAS, canned dry milk, canned fish, Cd, Cu, Pb, Zn

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698 MXene Quantum Dots Decorated Double-Shelled Ceo₂ Hollow Spheres for Efficient Electrocatalytic Nitrogen Oxidation

Authors: Quan Li, Dongcai Shen, Zhengting Xiao, Xin Liu Mingrui Wu, Licheng Liu, Qin Li, Xianguo Li, Wentai Wang

Abstract:

Direct electrocatalytic nitrogen oxidation (NOR) provides a promising alternative strategy for synthesizing high-value-added nitric acid from widespread N₂, which overcomes the disadvantages of the Haber-Bosch-Ostwald process. However, the NOR process suffers from the limitation of high N≡N bonding energy (941 kJ mol− ¹), sluggish kinetics, low efficiency and yield. It is a prerequisite to develop more efficient electrocatalysts for NOR. Herein, we synthesized double-shelled CeO₂ hollow spheres (D-CeO₂) and further modified with Ti₃C₂ MXene quantum dots (MQDs) for electrocatalytic N₂ oxidation, which exhibited a NO₃− yield of 71.25 μg h− ¹ mgcat− ¹ and FE of 31.80% at 1.7 V. The unique quantum size effect and abundant edge active sites lead to a more effective capture of nitrogen. Moreover, the double-shelled hollow structure is favorable for N₂ fixation and gathers intermediate products in the interlayer of the core-shell. The in-situ infrared Fourier transform spectroscopy confirmed the formation of *NO and NO₃− species during the NOR reaction, and the kinetics and possible pathways of NOR were calculated by density functional theory (DFT). In addition, a Zn-N₂ reaction device was assembled with D-CeO₂/MQDs as anode and Zn plate as cathode, obtaining an extremely high NO₃− yield of 104.57 μg h− ¹ mgcat− ¹ at 1 mA cm− ².

Keywords: electrocatalytic N₂ oxidation, nitrate production, CeO₂, MXene quantum dots, double-shelled hollow spheres

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697 Ultrasonic Techniques to Characterize and Monitor Water-in-Oil Emulsion

Authors: E. A. Alshaafi, A. Prakash

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Oil-water emulsions are commonly encountered in various industrial operations and at different stages of crude oil production and processing. Emulsions are often difficult to track and treat and can cause a number of costly problems which need to be avoided. The characteristics of the emulsion phase can vary with crude composition and types of impurities present in oil. The objectives of this study are the development of ultrasonic techniques to track and characterize emulsion phase generated during production and cleaning of crude oil. The position of emulsion layer is monitored with the help of ultrasonic probes suitably placed in the vessel. The sensitivity of the technique and its potential has been demonstrated based on extensive testing with different oil samples. The technique is also being developed to monitor emulsion phase characteristics such as stability, composition, and droplet size distribution. The ultrasonic parameters recorded are changes in acoustic velocity, signal attenuation and its frequency spectrum. Emulsion has been prepared with light mineral oil sample and the effects of various factors including mixing speed, temperature, surfactant, and solid particles concentrations have been investigated. The applied frequency for ultrasonic waves has been varied from 1 to 5 MHz to carry out a sensitivity analysis. Emulsion droplet structure is observed with optical microscopy and stability is examined by tracking the changes in ultrasonic parameters with time. A model based on ultrasonic attenuation spectroscopy is being developed and tested to track changes in droplet size distribution with time.

Keywords: ultrasonic techniques, emulsion, characterization, droplet size

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696 Micro-Arc Oxidation Titanium and Post Treatment by Cold Plasma and Graft Polymerization of Acrylic Acid for Biomedical Application

Authors: Shu-Chuan Liao, Chia-Ti Chang, Ko-Shao Chen

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Titanium and its alloy are widely used in many fields such as dentistry or orthopaedics. Due to their high strength low elastic modulus that chemical inertness and bio inert. The micro-arc oxidation used to formation a micro porous ceramic oxide layer film on Titanium surface and also to improve the resistance corrosion. For improving the biocompatibility, micro-arc oxidation surfaces bio-inert need to introduce reactive group. We introduced boundary layer by used plasma enhanced chemical vapor deposition of hexamethyldisilazane (HMDS) and organic active layer by UV light graft reactive monomer acrylic acid (AAc) therefore we can immobilize Chondroitin sulphate on surface easily by crosslinking EDC/NHS. The surface properties and composition of the modified layer were measured by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and water contact angle. Water contact angle of the plasma-treated Ti surface decreases from 60° to 38°, which is an indication of hydrophilicity. The results of electrochemical polarization analysis showed that the sample plasma treated at micro-arc oxidation after plasma treatment has the best corrosion resistance. The result showed that we can immobilize chondroitin sulfate successful by a series of modification and MTT assay indicated the biocompatibility has been improved in this study.

Keywords: MAO, plasma, graft polymerization, biomedical application

Procedia PDF Downloads 258
695 Fluorescence Quenching as an Efficient Tool for Sensing Application: Study on the Fluorescence Quenching of Naphthalimide Dye by Graphene Oxide

Authors: Sanaz Seraj, Shohre Rouhani

Abstract:

Recently, graphene has gained much attention because of its unique optical, mechanical, electrical, and thermal properties. Graphene has been used as a key material in the technological applications in various areas such as sensors, drug delivery, super capacitors, transparent conductor, and solar cell. It has a superior quenching efficiency for various fluorophores. Based on these unique properties, the optical sensors with graphene materials as the energy acceptors have demonstrated great success in recent years. During quenching, the emission of a fluorophore is perturbed by a quencher which can be a substrate or biomolecule, and due to this phenomenon, fluorophore-quencher has been used for selective detection of target molecules. Among fluorescence dyes, 1,8-naphthalimide is well known for its typical intramolecular charge transfer (ICT) and photo-induced charge transfer (PET) fluorophore, strong absorption and emission in the visible region, high photo stability, and large Stokes shift. Derivatives of 1,8-naphthalimides have found applications in some areas, especially fluorescence sensors. Herein, the fluorescence quenching of graphene oxide has been carried out on a naphthalimide dye as a fluorescent probe model. The quenching ability of graphene oxide on naphthalimide dye was studied by UV-VIS and fluorescence spectroscopy. This study showed that graphene is an efficient quencher for fluorescent dyes. Therefore, it can be used as a suitable candidate sensing platform. To the best of our knowledge, studies on the quenching and absorption of naphthalimide dyes by graphene oxide are rare.

Keywords: fluorescence, graphene oxide, naphthalimide dye, quenching

Procedia PDF Downloads 591
694 Design and Fabrication of ZSO Nanocomposite Thin Film Based NO2 Gas Sensor

Authors: Bal Chandra Yadav, Rakesh K. Sonker, Anjali Sharma, Punit Tyagi, Vinay Gupta, Monika Tomar

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In the present study, ZnO doped SnO2 thin films of various compositions were deposited on the surface of a corning substrate by dropping the two sols containing the precursors for composite (ZSO) with subsequent heat treatment. The sensor materials used for selective detection of nitrogen dioxide (NO2) were designed from the correlation between the sensor composition and gas response. The available NO2 sensors are operative at very high temperature (150-800 °C) with low sensing response (2-100) even in higher concentrations. Efforts are continuing towards the development of NO2 gas sensor aiming with an enhanced response along with a reduction in operating temperature by incorporating some catalysts or dopants. Thus in this work, a novel sensor structure based on ZSO nanocomposite has been fabricated using chemical route for the detection of NO2 gas. The structural, surface morphological and optical properties of prepared films have been studied by using X-ray diffraction (XRD), Atomic force microscopy (AFM), Transmission electron microscope (TEM) and UV-visible spectroscopy respectively. The effect of thickness variation from 230 nm to 644 nm of ZSO composite thin film has been studied and the ZSO thin film of thickness ~ 460 nm was found to exhibit the maximum gas sensing response ~ 2.1×103 towards 20 ppm NO2 gas at an operating temperature of 90 °C. The average response and recovery times of the sensor were observed to be 3.51 and 6.91 min respectively. Selectivity of the sensor was checked with the cross-exposure of vapour CO, acetone, IPA, CH4, NH3 and CO2 gases. It was found that besides the higher sensing response towards NO2 gas, the prepared ZSO thin film was also highly selective towards NO2 gas.

Keywords: ZSO nanocomposite thin film, ZnO tetrapod structure, NO2 gas sensor, sol-gel method

Procedia PDF Downloads 339
693 Malachite Ore Treatment with Typical Ammonium Salts and Its Mechanism to Promote the Flotation Performance

Authors: Ayman M. Ibrahim, Jinpeng Cai, Peilun Shen, Dianwen Liu

Abstract:

The difference in promoting sulfurization between different ammonium salts and its anion's effect on the sulfurization of the malachite surface was systematically studied. Therefore, this study takes malachite, a typical copper oxide mineral, as the research object, field emission scanning electron microscopy and energy-dispersive X-ray analysis (FESEM‒EDS), X-ray photoelectron spectroscopy (XPS), and other analytical and testing methods, as well as pure mineral flotation experiments, were carried out to examine the superiority of the ammonium salts as the sulfurizing reagent of malachite at the microscopic level. Additionally, the promoting effects of ammonium sulfate and ammonium phosphate on the malachite sulfurization of xanthate-flotation were compared systematically from the microstructure of sulfurized products, elemental composition, chemical state of characteristic elements, and hydrophobicity surface evolution. The FESEM and AFM results presented that after being pre-treated with ammonium salts, the adhesion of sulfurized products formed on the mineral surface was denser; thus, the flake radial dimension product was significantly greater. For malachite sulfurization flotation, the impact of ammonium phosphate in promoting sulfurization is weaker than ammonium sulfate. The reason may be that hydrolyzing phosphate consumes a substantial quantity of H+ in the solution, which hastens the formation of the copper-sulfur products, decreasing the adhesion stability of copper-sulfur species on the malachite surface.

Keywords: sulfurization flotation, adsorption characteristics, malachite, hydrophobicity

Procedia PDF Downloads 67
692 Tailoring Polycrystalline Diamond for Increasing Earth-Drilling Challenges

Authors: Jie Chen, Chris Cheng, Kai Zhang

Abstract:

Polycrystalline diamond compact (PDC) cutters with a polycrystalline diamond (PCD) table supported by a cemented tungsten carbide substrate have been widely used for earth-drilling tools in the oil and gas industry. Both wear and impact resistances are key figure of merits of PDC cutters, and they are closely related to the microstructure of the PCD table. As oil and gas exploration enters deeper, harder, and more complex formations, plus increasing requirement of accelerated downhole drilling speed and drilling cost reduction, current PDC cutters face unprecedented challenges for maintaining a longer drilling life than ever. Excessive wear on uneven hard formations, spalling, chipping, and premature fracture due to impact loads are common failure modes of PDC cutters in the field. Tailoring microstructure of the PCD table is one of the effective approaches to improve the wear and impact resistances of PDC cutters, along with other factors such as cutter geometry and bit design. In this research, cross-sectional microstructure, fracture surface, wear surface, and elemental composition of PDC cutters were analyzed using scanning electron microscopy (SEM) with both backscattered electron and secondary electron detectors, and energy dispersive X-ray spectroscopy (EDS). The microstructure and elemental composition were further correlated with the wear and impact resistances of corresponding PDC cutters. Wear modes and impact toughening mechanisms of state-of-the-art PDCs were identified. Directions to further improve the wear and impact resistances of PDC cutters were proposed.

Keywords: fracture surface, microstructure, polycrystalline diamond, PDC, wear surface

Procedia PDF Downloads 53
691 Synthesis and Characterization of Un-Doped and Velvet Tamarind Doped ZnS Crystals, Using Sol Gel Method

Authors: Uchechukwu Vincent Okpala

Abstract:

Under the Sun, energy is a key factor for the sustenance of life and its environment. The need to protect the environment as energy is generated and consumed has called for renewable and green energy sources. To be part of this green revolution, we synthesized and characterized undoped and velvet tamarind doped zinc sulfide (ZnS) crystals using sol-gel methods. Velvet tamarind was whittled down using the top-down approach of nanotechnology. Sodium silicate, tartaric acid, zinc nitrate, and thiourea were used as precursors. The grown samples were annealed at 105°C. Structural, optical, and compositional analyses of the grown samples revealed crystalline structures with varied crystallite sizes influenced by doping. Energy-dispersive X-ray spectroscopy confirmed elemental compositions of Zn, S, C and O in the films. Atomic percentages of the elements varied with VT doping. FT-IR analysis indicated the presence of functional groups like O-H stretching (alcohol), C=C=C stretching (alkene group), C=C bending, C-H stretching (alkane), N-H stretching (aliphatic primary amine) and N=C=S stretching (isothiocyanate) constituent in the film. The transmittance of the samples increased from the visible region to the infrared region making the samples good for poultry and solar energy applications. The bandgap energy of the films decreased as the number of VT drops increased, from 2.4 to 2.2. They were wide band gap materials and were good for optoelectronic, photo-thermal, high temperature, high power and solar cell applications.

Keywords: doping, sol-gel, velvet tamarind, ZnS.

Procedia PDF Downloads 47
690 Effect of Plasma Treatment on UV Protection Properties of Fabrics

Authors: Sheila Shahidi

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UV protection by fabrics has recently become a focus of great interest, particularly in connection with environmental degradation or ozone layer depletion. Fabrics provide simple and convenient protection against UV radiation (UVR), but not all fabrics offer sufficient UV protection. To describe the degree of UVR protection offered by clothing materials, the ultraviolet protection factor (UPF) is commonly used. UV-protective fabric can be generated by application of a chemical finish using normal wet-processing methodologies. However, traditional wet-processing techniques are known to consume large quantities of water and energy and may lead to adverse alterations of the bulk properties of the substrate. Recently, usage of plasmas to generate physicochemical surface modifications of textile substrates has become an intriguing approach to replace or enhance conventional wet-processing techniques. In this research work the effect of plasma treatment on UV protection properties of fabrics was investigated. DC magnetron sputtering was used and the parameters of plasma such as gas type, electrodes, time of exposure, power and, etc. were studied. The morphological and chemical properties of samples were analyzed using Scanning Electron Microscope (SEM) and Furrier Transform Infrared Spectroscopy (FTIR), respectively. The transmittance and UPF values of the original and plasma-treated samples were measured using a Shimadzu UV3101 PC (UV–Vis–NIR scanning spectrophotometer, 190–2, 100 nm range). It was concluded that, plasma which is an echo-friendly, cost effective and dry technique is being used in different branches of the industries, and will conquer textile industry in the near future. Also it is promising method for preparation of UV protection textile.

Keywords: fabric, plasma, textile, UV protection

Procedia PDF Downloads 519
689 Enhancing Cellulose Acetate Films: Impact of Glycerol and Ionic Liquid Plasticizers

Authors: Rezzouq Asiya, Bouftou Abderrahim, Belfadil Doha, Taoufyk Azzeddine, El Bouchti Mehdi, Zyade Souad, Cherkaoui Omar, Majid Sanaa

Abstract:

Plastic packaging is widely used, but its pollution is a major environmental problem. Solutions require new sustainable technologies, environmental management, and the use of bio-based polymers as sustainable packaging. Cellulose acetate (CA) is a biobased polymer used in a variety of applications such as the manufacture of plastic films, textiles, and filters. However, it has limitations in terms of thermal stability and rigidity, which necessitates the addition of plasticizers to optimize its use in packaging. Plasticizers are molecules that increase the flexibility of polymers, but their influence on the chemical and physical properties of films (CA) has not been studied in detail. Some studies have focused on mechanical and thermal properties. However, an in-depth analysis is needed to understand the interactions between the additives and the polymer matrix. In this study, the aim is to examine the effect of two types of plasticizers, glycerol (a conventional plasticizer) and an ionic liquid, on the transparency, mechanical, thermal and barrier properties of cellulose acetate (CA) films prepared by the solution-casting method . Various analytical techniques were used to characterize these films, including infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), water vapor permeability (WVP), oxygen permeability, scanning electron microscopy (SEM), opacity, transmission analysis and mechanical tests.

Keywords: cellulose acetate, plasticizers, biopolymers, ionic liquid, glycerol.

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688 Study of Corrosion Behavior of Experimental Alloys with Different Levels of Cr and High Levels of Mo Compared to Aisi 444

Authors: Ana P. R. N. Barroso, Maurício N. Kleinberg, Frederico R. Silva, Rodrigo F. Guimarães, Marcelo M. V. Parente, Walney S. Araújo

Abstract:

The fight against accelerated wear of the equipment used in the oil and gas sector is a challenge for minimizing maintenance costs. Corrosion being one of the main agents of equipment deterioration, we seek alternative materials that exhibit improved corrosion resistance at low cost of production. This study aims to evaluate the corrosion behavior of experimental alloys containing 15% and 17% of chromium (Cr) and 5% of molybdenum (Mo) in comparison with an AISI 444 commercial alloy. Microstructural analyzes were performed on samples of the alloys before and after the electrochemical tests. Two samples of each solubilized alloy were also taken for analysis of the corrosion behavior by testing potentiodynamic polarization (PP) and Electrochemical Impedance Spectroscopy (EIS) with immersion time of 24 hours in electrolytic solution with acidic character. The graphics obtained through electrochemical tests of PP and EIS indicated that among the experimental alloys, the alloy with higher chromium content (17%) had a higher corrosion resistance, confirming the beneficial effect of adding chromium. When comparing the experimental alloys with the AISI 444 commercial alloy, it is observed that the AISI 444 commercial alloy showed superior corrosion resistance to that of the experimental alloys for both assays, PP and EIS. The microstructural analyzes performed after the PP and EIS tests confirmed the results previously described. These results suggest that the addition of these levels of molybdenum did not favor the electrochemical behavior of experimental ferritic alloys for the electrolytic medium studied.

Keywords: corrosion, molybdenum, electrochemical tests, experimental alloys

Procedia PDF Downloads 573
687 [Keynote Talk]: Determination of Metal Content in the Surface Sediments of the Istanbul Bosphorus Strait

Authors: Durata Haciu, Elif Sena Tekin, Gokce Ozturk, Patricia Ramey Balcı

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Coastal zones are under increasing threat due to anthropogenic activities that introduce considerable pollutants such as heavy metals into marine ecosystems. As part of a larger experimental study examining species responses to contaminated marine sediments, surface sediments (top 5cm) were analysed for major trace elements at three locations in Istanbul Straight. Samples were randomly collected by divers (May 2018) using hand-corers from Istinye (n=4), Garipce (n=10) and Poyrazköy (n=6), at water depths of 4-8m. Twelve metals were examined: As, arsenic; Pb, lead; Cd, cadmium; Cr, chromium; Cu, Copper; Fe, Iron; Ni, Nickel; Zn, Zinc; V, vanadium; Mn, Manganese; Ba, Barium; and Ag, silver by wavelength-dispersive X-ray fluorescence spectrometry (WDXRF) and Inductively Coupled Plasma/Mass Spectroscopy (ICP/MS). Preliminary results indicate that the average concentrations of metals (mg kg⁻¹) varied considerably among locations. In general, concentrations were relatively lower at Garipce compared to either Istinye or Poyrazköy. For most metals mean concentrations were highest at Poyrazköy and Ag and Cd were below detection limits (exception= Ag in a few samples). While Cd and As were undetected in all stations, the concentrations of Fe and Ni fall in the criteria of moderately polluted range and the rest of the metals in the range of low polluted range as compared to Effects Range Low (ERL) and Effects Range median (ERM) values determined by US Environmental Protection Agency (EPA).

Keywords: effect-range classification, ICP/MS, marine sediments, XRF

Procedia PDF Downloads 131