Search results for: copper-infused magnesium hydroxide
Commenced in January 2007
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Edition: International
Paper Count: 585

Search results for: copper-infused magnesium hydroxide

435 Optimal Consume of NaOH in Starches Gelatinization for Froth Flotation

Authors: André C. Silva, Débora N. Sousa, Elenice M. S. Silva, Thales P. Fontes, Raphael S. Tomaz

Abstract:

Starches are widely used as depressant in froth flotation operations in Brazil due to their efficiency, increasing the selectivity in the inverse flotation of quartz depressing iron ore. Starches market have been growing and improving in recent years, leading to better products attending the requirements of the mineral industry. The major source of starch used for iron ore is corn starch, which needs to be gelatinized with sodium hydroxide (NaOH) prior to use. This stage has a direct impact on industrials costs, once the lowest consumption of NaOH in gelatinization provides better control of the pH in the froth flotation and reduces the amount of electrolytes present in the pulp. In order to evaluate the gelatinization degree of different starches and flour were subjected to the addiction of NaOH and temperature variation experiments. Samples of starch (corn, cassava, HIPIX 100, HIPIX 101 and HIPIX 102 commercialized by Ingredion) and flour (cassava and potato) were tested. The starch samples were characterized through Scanning Electronic Microscopy and the amylose content were determined through spectrometry, swelling and solubility tests. The gelatinization was carried out through titration with NaOH, keeping the solution temperature constant at 40 oC. At the end of the tests, the optimal amount of NaOH consumed to gelatinize the starch or flour from different botanical sources was established and a correlation between the content of amylopectin in the starch and the starch/NaOH ratio needed for its gelatinization.

Keywords: froth flotation, gelatinization, sodium hydroxide, starches and flours

Procedia PDF Downloads 333
434 Ecosystem Restoration: Remediation of Crude Oil-Polluted Soil by Leuceana leucocephala (Lam.) de Wit

Authors: Ayodele Adelusi Oyedeji

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The study was carried out under a controlled environment with the aim of examining remediation of crude oil polluted soil. The germination rate, heights and girths, number of leaves and nodulation was determined following standard procedures. Some physicochemical (organic matter, pH, nitrogen, phosphorous, potassium, calcium, magnesium and sodium) characteristics of soil used were determined using standard protocols. Results showed that at varying concentration of crude oil i.e 0 ml, 25 ml, 50 ml, 75 ml and 100 ml, Leuceana leucocephala had germination rate of 92%, 90%, 84%, 62% and 56% respectively, mean height of 73.70cm, 58.30cm, 49.50cm, 46.45cm and 41.80cm respectively after 16 weeks after planting (WAP), mean girth of 0.54mm, 0.34mm, 0.33mm, 0.21mm and 0.19mm respectively at 16 WAP, number of nodules 18, 10, 10, 6 and 2 respectively and number of leaves 24.00, 16.00, 13.00, 10.00 and 6.00 respectively. The organic matter, pH, nitrogen, phosphorous, potassium, calcium, magnesium, and sodium decreased with the increase in the concentration of crude oil. Furthermore, as the concentration of crude oil increased the germination rate, height, girth, and number of leaves and nodules decreased, suggesting the effect of crude oil on Leuceana leucocephala. The plant withstands the varying concentration of the crude oil means that it could be used for the remediation of crude oil contaminated soil in the Niger Delta region of Nigeria.

Keywords: ecosystem conservation, Leuceana leucocephala, phytoremediation, soil pollution

Procedia PDF Downloads 81
433 Optimization of Chitosan Membrane Production Parameters for Zinc Ion Adsorption

Authors: Peter O. Osifo, Hein W. J. P. Neomagus, Hein V. D. Merwe

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Chitosan materials from different sources of raw materials were characterized in order to determine optimal preparation conditions and parameters for membrane production. The membrane parameters such as molecular weight, viscosity, and degree of deacetylation were used to evaluate the membrane performance for zinc ion adsorption. The molecular weight of the chitosan was found to influence the viscosity of the chitosan/acetic acid solution. An increase in molecular weight (60000-400000 kg.kmol-1) of the chitosan resulted in a higher viscosity (0.05-0.65 Pa.s) of the chitosan/acetic acid solution. The effect of the degree of deacetylation on the viscosity is not significant. The effect of the membrane production parameters (chitosan- and acetic acid concentration) on the viscosity is mainly determined by the chitosan concentration. For higher chitosan concentrations, a membrane with a better adsorption capacity was obtained. The membrane adsorption capacity increases from 20-130 mg Zn per gram of wet membrane for an increase in chitosan concentration from 2-7 mass %. Chitosan concentrations below 2 and above 7.5 mass % produced membranes that lack good mechanical properties. The optimum manufacturing conditions including chitosan concentration, acetic acid concentration, sodium hydroxide concentration and crosslinking for chitosan membranes within the workable range were defined by the criteria of adsorption capacity and flux. The adsorption increases (50-120 mg.g-1) as the acetic acid concentration increases (1-7 mass %). The sodium hydroxide concentration seems not to have a large effect on the adsorption characteristics of the membrane however, a maximum was reached at a concentration of 5 mass %. The adsorption capacity per gram of wet membrane strongly increases with the chitosan concentration in the acetic acid solution but remains constant per gram of dry chitosan. The optimum solution for membrane production consists of 7 mass % chitosan and 4 mass % acetic acid in de-ionised water. The sodium hydroxide concentration for phase inversion is at optimum at 5 mass %. The optimum cross-linking time was determined to be 6 hours (Percentage crosslinking of 18%). As the cross-linking time increases the adsorption of the zinc decreases (150-50 mg.g-1) in the time range of 0 to 12 hours. After a crosslinking time of 12 hours, the adsorption capacity remains constant. This trend is comparable to the effect on flux through the membrane. The flux decreases (10-3 L.m-2.hr-1) with an increase in crosslinking time range of 0 to 12 hours and reaches a constant minimum after 12 hours.

Keywords: chitosan, membrane, waste water, heavy metal ions, adsorption

Procedia PDF Downloads 354
432 Association of Phosphorus and Magnesium with Fat Indices in Children with Metabolic Syndrome

Authors: Mustafa M. Donma, Orkide Donma

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Metabolic syndrome (MetS) is a disease associated with obesity. It is a complicated clinical problem possibly affecting body composition as well as macrominerals. These parameters gain further attention, particularly in the pediatric population. The aim of this study is to investigate the amount of discrete body composition fractions in groups that differ in the severity of obesity. Also, the possible associations with calcium (Ca), phosphorus (P), magnesium (Mg) will be examined. The study population was divided into four groups. Twenty-eight, 29, 34, and 34 children were involved in Group 1 (healthy), 2 (obese), 3 (morbid obese), and 4 (MetS), respectively. Institutional Ethical Committee approved the study protocol. Informed consent forms were obtained from the participants. The classification of obese groups was performed based upon the recommendations of the World Health Organization. Metabolic syndrome components were defined. Serum Ca, P, Mg concentrations were measured. Within the scope of body composition, fat mass, fat-free mass, protein mass, mineral mass were determined by a body composition monitor using bioelectrical impedance analysis technology. Weight, height, waist circumference, hip circumference, head circumference, and neck circumference values were recorded. Body mass index, diagnostic obesity notation model assessment index, fat mass index, and fat-free mass index values were calculated. Data were statistically evaluated and interpreted. There was no statistically significant difference among the groups in terms of Ca and P concentrations. Magnesium concentrations differed between Group 1 and Group 4. Strong negative correlations were detected between P as well as Mg and fat mass index as well as diagnostic obesity notation model assessment index in Group 4, the group, which comprised morbid obese children with MetS. This study emphasized unique associations of P and Mg minerals with diagnostic obesity notation model assessment index and fat mass index during the evaluation of morbid obese children with MetS. It was also concluded that diagnostic obesity notation model assessment index and fat mass index were more proper indices in comparison with body mass index and fat-free mass index for the purpose of defining body composition in children.

Keywords: children, fat mass, fat-free mass, macrominerals, obesity

Procedia PDF Downloads 127
431 Effect of Magnesium Inoculation on the Microstructure and Mechanical Properties of a Spheroidal Cast Iron Knuckle: A Focus on the Steering Arm

Authors: Steven Mavhungu, Didier Nyembwe, Daniel Sekotlong

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The steering knuckle is an integral component of the suspension and stability control system of modern vehicles. Good mechanical properties with an emphasis on the fatigue properties are essential for this component as it is subjected to cyclical load of significant magnitude during service. These properties are a function of the microstructure achieved in the component during the various manufacturing processes including forging and casting. The strut mount of the knuckle is required to meet specified microstructure and mechanical properties. However, in line with the recent trend of stringent quality requirements of cast components, Original Equipment Manufacturers (OEMs) have had to extend the specifications to other sections of the knuckle. This paper evaluates the effect of cored wire inoculation on the microstructure and mechanical properties of the steering arm of a typical spheroidal cast iron component. The investigation shows that the use of a cored wire having higher rare earth content formulation could possibly lead to a homogeneous matrix containing consistent graphite nodule morphology. However, this was found not to be the condition for better mechanical properties along the knuckle arm in line with required specifications. The findings in this paper contribute to a better understanding of steering knuckle properties to allow its production for safer automobile applications.

Keywords: inoculation, magnesium cored wire, spheroidal graphie, steering knuckle

Procedia PDF Downloads 195
430 Removal of Heavy Metals by KOH Activated Diplotaxis harra Biomass: Experimental Design Optimization

Authors: H. Tounsadi, A. Khalidi, M. Abdennouri, N. Barka

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The objective of this study was to produce high quality activated carbons from Diplotaxis harra biomass by potassium hydroxide activation and their application for heavy metals removal. To reduce the number of experiments, full factorial experimental design at two levels were carried out to occur optimal preparation conditions and better conditions for the removal of cadmium and cobalt ions from aqueous solutions. The influence of different variables during the activation process, such as carbonization temperature, activation temperature, activation time and impregnation ratio (g KOH/g carbon) have been investigated, and the best production conditions were determined. The experimental results showed that removal of cadmium and cobalt ions onto activated carbons was more sensitive to methylene blue index instead of iodine number. Although, the removal of cadmium and cobalt ions is more influenced by activation temperature with a negative effect followed by the impregnation ratio with a positive impact. Based on the statistical data, the best conditions for the removal of cadmium and cobalt by prepared activated carbons have been established. The maximum iodine number and methylene blue index obtained under these conditions and the greater sorption capacities for cadmium and cobalt were investigated. These sorption capacities were greater than those of a commercial activated carbon used in water treatment.

Keywords: activated carbon, cadmium, cobalt, Diplotaxis harra, experimental design, potassium hydroxide

Procedia PDF Downloads 172
429 Improving Enhanced Oil Recovery by Using Alkaline-Surfactant-Polymer Injection and Nanotechnology

Authors: Amir Gerayeli, Babak Moradi

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The continuously declining oil reservoirs and reservoirs aging have created a huge demand for utilization of Enhanced Oil Recovery (EOR) methods recently. Primary and secondary oil recovery methods have various limitations and are not practical for all reservoirs. Therefore, it is necessary to use chemical methods to improve oil recovery efficiency by reducing oil and water surface tension, increasing sweeping efficiency, and reducing displacer phase viscosity. One of the well-known methods of oil recovery is Alkaline-Surfactant-Polymer (ASP) flooding that shown to have significant impact on enhancing oil recovery. As some of the biggest oil reservoirs including those of Iran’s are fractional reservoirs with substantial amount of trapped oil in their fractures, the use of Alkaline-Surfactant-Polymer (ASP) flooding method is increasingly growing, the method in which the impact of several parameters including type and concentration of the Alkaline, Surfactant, and polymer are particularly important. This study investigated the use of Nano particles to improve Enhanced Oil Recovery (EOR). The study methodology included performing several laboratory tests on drill cores extracted from Karanj Oil field Asmary Formation in Khuzestan, Iran. In the experiments performed, Sodium dodecyl benzenesulfonate (SDBS) and 1-dodecyl-3-methylimidazolium chloride ([C12mim] [Cl])) were used as surfactant, hydrolyzed polyacrylamide (HPAM) and guar gum were used as polymer, Sodium hydroxide (NaOH) as alkaline, and Silicon dioxide (SiO2) and Magnesium oxide (MgO) were used as Nano particles. The experiment findings suggest that water viscosity increased from 1 centipoise to 5 centipoise when hydrolyzed polyacrylamide (HPAM) and guar gum were used as polymer. The surface tension between oil and water was initially measured as 25.808 (mN/m). The optimum surfactant concentration was found to be 500 p, at which the oil and water tension surface was measured to be 2.90 (mN/m) when [C12mim] [Cl] was used, and 3.28 (mN/m) when SDBS was used. The Nano particles concentration ranged from 100 ppm to 1500 ppm in this study. The optimum Nano particle concentration was found to be 1000 ppm for MgO and 500 ppm for SiO2.

Keywords: alkaline-surfactant-polymer, ionic liquids, relative permeability, reduced surface tension, tertiary enhanced oil recovery, wettability change

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428 “BUM629” Special Hybrid Reinforcement Materials for Mega Structures

Authors: Gautam, Arjun, V. R. Sharma

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In the civil construction steel and concrete plays a different role but the same purposes dealing with the design of structures that support or resist loads. Concrete has been used in construction since long time from now. Being brittle and weak in tension, concrete is always reinforced with steel bars for the purposes in beams and columns etc. The paper deals with idea of special designed 3D materials which we named as “BUM629” to be placed/anchored in the structural member and mixed with concrete later on, so as to resist the developments of cracks due to shear failure , buckling,tension and compressive load in concrete. It had cutting edge technology through Draft, Analysis and Design the “BUM629”. The results show that “BUM629” has the great results in Mechanical application. Its material properties are design according to the need of structure; we apply the material such as Mild Steel and Magnesium Alloy. “BUM629” are divided into two parts one is applied at the middle section of concrete member where bending movements are maximum and the second part is laying parallel to vertical bars near clear cover, so we design this material and apply in Reinforcement of Civil Structures. “BUM629” is analysis and design for use in the mega structures like skyscrapers, dams and bridges.

Keywords: BUM629, magnesium alloy, cutting edge technology, mechanical application, draft, analysis and design, mega structures

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427 Potentiostatic Growth of Hazenite Mineral Coating on AZ31 Magnesium Alloy in 0.1 M K₂HPO₄/0.1 M Na₂HPO₄ Solution

Authors: Liping Wu, Durga Bhakta Pokharel, Junhua Dong, Changgang Wang, Lin Zhao, Wei Ke, Nan Chen

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Hazenite conversion coating was deposited on AZ31 Mg alloy in a deaerated phosphate solution containing 0.1 M K₂HPO₄ and 0.1 M Na₂HPO₄ (Na₀.₁K0₀.₁) with pH 9 at −0.8 V. The coating mechanism of hazenite was elucidated by in situ potentiostatic current decay, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), electron probe micro-analyzer (EPMA) and differential scanning calorimetry (DSC). The volume of H₂ evolved during potentiostatic polarization was measured by a gas collection apparatus. The degradation resistance of the hazenite coating was evaluated in simulated body fluid (SBF) at 37℃ by using potentiodynamic polarization (PDP). The results showed that amorphous Mg(OH)₂ was deposited first, followed by the transformation of Mg(OH)₂ to amorphous MgHPO₄, subsequently the conversion of MgHPO₄ to crystallized K-struvite (KMgPO₄·6H₂O), finally the crystallization of crystallized hazenite (NaKMg₂(PO₄)₂·14H₂O). The deposited coating was composed of four layers where the inner layer is comprised of Mg(OH)₂, the middle layer of Mg(OH)₂ and MgHPO₄, the top layer of Mg(OH)₂, MgHPO₄ and K-struvite, the topmost layer of Mg(OH)₂, MgHPO₄, K-struvite and hazenite (NaKMg₂(PO₄)₂·14H₂O). The PD results showed that the hazenite coating decreased the corrosion rate by two orders of magnitude.

Keywords: magnesium alloy, potentiostatic technique, hazenite, mineral conversion coating

Procedia PDF Downloads 144
426 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

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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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425 Non Destructive Ultrasound Testing for the Determination of Elastic Characteristics of AlSi7Zn3Cu2Mg Foundry Alloy

Authors: A. Hakem, Y. Bouafia

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Characterization of materials used for various mechanical components is of great importance in their design. Several studies were conducted by various authors in order to improve their physical and/or chemical properties in general and mechanical or metallurgical properties in particular. The foundry alloy AlSi7Zn3Cu2Mg is one of the main components constituting the various mechanisms for the implementation of applications and various industrial projects. Obtaining a reliable product is not an easy task; several results proposed by different authors show sometimes results that can contradictory. Due to their high mechanical characteristics, these alloys are widely used in engineering. Silicon improves casting properties and magnesium allows heat treatment. It is thus possible to obtain various degrees of hardening and therefore interesting compromise between tensile strength and yield strength, on one hand, and elongation, on the other hand. These mechanical characteristics can be further enhanced by a series of mechanical treatments or heat treatments. Their light weight coupled with high mechanical characteristics, aluminum alloys are very much used in cars and aircraft industry. The present study is focused on the influence of heat treatments which cause significant micro structural changes, usually hardening by variation of annealing temperatures by increments of 10°C and 20°C on the evolution of the main elastic characteristics, the resistance, the ductility and the structural characteristics of AlSi7Zn3Cu2Mg foundry alloy cast in sand by gravity. These elastic properties are determined in three directions for each specimen of dimensions 200x150x20 mm³ by the ultrasonic method based on acoustic or elastic waves. The hardness, the micro hardness and the structural characteristics are evaluated by a non-destructive method. The aim of this work is to study the hardening ability of AlSi7Zn3Cu2Mg alloy by considering ten states. To improve the mechanical properties obtained with the raw casting, one should use heat treatment for structural hardening; the addition of magnesium is necessary to increase the sensitivity to this specific heat treatment: Treatment followed by homogenization which generates a diffusion of atoms in a substitution solid solution inside a hardening furnace at 500°C during 8h, followed immediately by quenching in water at room temperature 20 to 25°C, then an ageing process for 17h at room temperature and at different annealing temperature (150, 160, 170, 180, 190, 240, 200, 220 and 240°C) for 20h in an annealing oven. The specimens were allowed to cool inside the oven.

Keywords: aluminum, foundry alloy, magnesium, mechanical characteristics, silicon

Procedia PDF Downloads 236
424 The Effects and Interactions of Synthesis Parameters on Properties of Mg Substituted Hydroxyapatite

Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

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In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the as-synthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p < 0.0001, two way Anova), however, these were independent of TEA addition (p > 0.15, two way Anova). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p < 0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way analysis of variance (ANOVA)

Procedia PDF Downloads 342
423 Batch and Dynamic Investigations on Magnesium Separation by Ion Exchange Adsorption: Performance and Cost Evaluation

Authors: Mohamed H. Sorour, Hayam F. Shaalan, Heba A. Hani, Eman S. Sayed

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Ion exchange adsorption has a long standing history of success for seawater softening and selective ion removal from saline sources. Strong, weak and mixed types ion exchange systems could be designed and optimized for target separation. In this paper, different types of adsorbents comprising zeolite 13X and kaolin, in addition to, poly acrylate/zeolite (AZ), poly acrylate/kaolin (AK) and stand-alone poly acrylate (A) hydrogel types were prepared via microwave (M) and ultrasonic (U) irradiation techniques. They were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The developed adsorbents were evaluated on bench scale level and based on assessment results, a composite bed has been formulated for performance evaluation in pilot scale column investigations. Owing to the hydrogel nature of the partially crosslinked poly acrylate, the developed adsorbents manifested a swelling capacity of about 50 g/g. The pilot trials have been carried out using magnesium enriched Red Seawater to simulate Red Seawater desalination brine. Batch studies indicated varying uptake efficiencies, where Mg adsorption decreases according to the following prepared hydrogel types AU>AM>AKM>AKU>AZM>AZU, being 108, 107, 78, 69, 66 and 63 mg/g, respectively. Composite bed adsorbent tested in the up-flow mode column studies indicated good performance for Mg uptake. For an operating cycle of 12 h, the maximum uptake during the loading cycle approached 92.5-100 mg/g, which is comparable to the performance of some commercial resins. Different regenerants have been explored to maximize regeneration and minimize the quantity of regenerants including 15% NaCl, 0.1 M HCl and sodium carbonate. Best results were obtained by acidified sodium chloride solution. In conclusion, developed cation exchange adsorbents comprising clay or zeolite support indicated adequate performance for Mg recovery under saline environment. Column design operated at the up-flow mode (approaching expanded bed) is appropriate for such type of separation. Preliminary cost indicators for Mg recovery via ion exchange have been developed and analyzed.

Keywords: batch and dynamic magnesium separation, seawater, polyacrylate hydrogel, cost evaluation

Procedia PDF Downloads 111
422 The Scanning Vibrating Electrode Technique (SVET) as a Tool for Optimising a Printed Ni(OH)2 Electrode under Charge Conditions

Authors: C. F. Glover, J. Marinaccio, A. Barnes, I. Mabbett, G. Williams

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The aim of the current study is to optimise formulations, in terms of charging efficiency, of a printed Ni(OH)2 precursor coating of a battery anode. Through the assessment of the current densities during charging, the efficiency of a range of formulations are compared. The Scanning vibrating electrode technique (SVET) is used extensively in the field of corrosion to measure area-averaged current densities of freely-corroding metal surfaces when fully immersed in electrolyte. Here, a Ni(OH)2 electrode is immersed in potassium hydroxide (30% w/v solution) electrolyte and charged using a range of applied currents. Samples are prepared whereby multiple coatings are applied to one substrate, separated by a non-conducting barrier, and charged using a constant current. With a known applied external current, electrode efficiencies can be calculated based on the current density outputs measured using SVET. When fully charged, a green Ni(OH)2 is oxidised to a black NiOOH surface. Distinct regions displaying high current density, and hence a faster oxidising reaction rate, are located using the SVET. This is confirmed by a darkening of the region upon transition to NiOOH. SVET is a highly effective tool for assessing homogeneity of electrodes during charge/discharge. This could prove particularly useful for electrodes where there are no visible surface appearance changes. Furthermore, a scanning Kelvin probe technique, traditionally used to assess underfilm delamination of organic coatings for the protection of metallic surfaces, is employed to study the change in phase of oxides, pre and post charging.

Keywords: battery, electrode, nickel hydroxide, SVET, printed

Procedia PDF Downloads 204
421 Magnesium Nanoparticles for Photothermal Therapy

Authors: E. Locatelli, I. Monaco, R. C. Martin, Y. Li, R. Pini, M. Chiariello, M. Comes Franchini

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Despite the many advantages of application of nanomaterials in the field of nanomedicine, increasing concerns have been expressed on their potential adverse effects on human health. There is urgency for novel green strategies toward novel materials with enhanced biocompatibility using safe reagents. Photothermal ablation therapy, which exploits localized heat increase of a few degrees to kill cancer cells, has appeared recently as a non-invasive and highly efficient therapy against various cancer types; anyway new agents able to generate hyperthermia when irradiated are needed and must have precise biocompatibility in order to avoid damage to healthy tissues and prevent toxicity. Recently, there has been increasing interest in magnesium as a biomaterial: it is the fourth most abundant cation in the human body, and it is essential for human metabolism. However magnesium nanoparticles (Mg NPs) have had limited diffusion due to the high reduction potential of magnesium cations, which makes NPs synthesis challenging. Herein, we report the synthesis of Mg NPs and their surface functionalization for the obtainment of a stable and biocompatible nanomaterial suitable for photothermal ablation therapy against cancer. We synthesized the Mg crystals by reducing MgCl2 with metallic lithium and exploiting naphthalene as an electron carrier: the lithium–naphthalene complex acts as the real reducing agent. Firstly, the nanocrystal particles were coated with the ligand 12-ethoxy ester dodecanehydroxamic acid, and then entrapped into water-dispersible polymeric micelles (PMs) made of the FDA-approved PLGA-b-PEG-COOH copolymer using the oil-in-water emulsion technique. Lately, we developed a more straightforward methodology by introducing chitosan, a highly biocompatible natural product, at the beginning of the process, simultaneously using lithium–naphthalene complex, thus having a one-pot procedure for the formation and surface modification of MgNPs. The obtained MgNPs were purified and fully characterized, showing diameters in the range of 50-300 nm. Notably, when coated with chitosan the particles remained stable as dry powder for more than 10 months. We proved the possibility of generating a temperature rise of a few to several degrees once MgNPs were illuminated using a 810 nm diode laser operating in continuous wave mode: the temperature rise resulted significant (0-15 °C) and concentration dependent. We then investigated potential cytotoxicity of the MgNPs: we used HN13 epithelial cells, derived from a head and neck squamous cell carcinoma and the hepa1-6 cell line, derived from hepatocellular carcinoma and very low toxicity was observed for both nanosystems. Finally, in vivo photothermal therapy was performed on xenograft hepa1-6 tumor bearing mice: the animals were treated with MgNPs coated with chitosan and showed no sign of suffering after the injection. After 12 hours the tumor was exposed to near-infrared laser light. The results clearly showed an extensive damage to tumor tissue after only 2 minutes of laser irradiation at 3Wcm-1, while no damage was reported when the tumor was treated with the laser and saline alone in control group. Despite the lower photothermal efficiency of Mg with respect to Au NPs, we consider MgNPs a promising, safe and green candidate for future clinical translations.

Keywords: chitosan, magnesium nanoparticles, nanomedicine, photothermal therapy

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420 Practical Method for Failure Prediction of Mg Alloy Sheets during Warm Forming Processes

Authors: Sang-Woo Kim, Young-Seon Lee

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An important concern in metal forming, even at elevated temperatures, is whether a desired deformation can be accomplished without any failure of the material. A detailed understanding of the critical condition for crack initiation provides not only the workability limit of a material but also a guide-line for process design. This paper describes the utilization of ductile fracture criteria in conjunction with the finite element method (FEM) for predicting the onset of fracture in warm metal working processes of magnesium alloy sheets. Critical damage values for various ductile fracture criteria were determined from uniaxial tensile tests and were expressed as the function of strain rate and temperature. In order to find the best criterion for failure prediction, Erichsen cupping tests under isothermal conditions and FE simulations combined with ductile fracture criteria were carried out. Based on the plastic deformation histories obtained from the FE analyses of the Erichsen cupping tests and the critical damage value curves, the initiation time and location of fracture were predicted under a bi-axial tensile condition. The results were compared with experimental results and the best criterion was recommended. In addition, the proposed methodology was used to predict the onset of fracture in non-isothermal deep drawing processes using an irregular shaped blank, and the results were verified experimentally.

Keywords: magnesium, AZ31 alloy, ductile fracture, FEM, sheet forming, Erichsen cupping test

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419 Mechanical Properties of Powder Metallurgy Processed Biodegradable Zn-Based Alloy for Biomedical Application

Authors: Maruf Yinka Kolawole, Jacob Olayiwola Aweda, Farasat Iqbal, Asif Ali, Sulaiman Abdulkareem

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Zinc is a non-ferrous metal with potential application in orthopaedic implant materials. However, its poor mechanical properties were major challenge to its application. Therefore, this paper studies the mechanical properties of biodegradable Zn-based alloy for biomedical application. Pure zinc powder with varying (0, 1, 2, 3 & 6) wt% of magnesium powders were ball milled using ball-to-powder ratio (B:P) of 10:1 at 350 rpm for 4 hours. The resulting milled powders were compacted and sintered at 300 MPa and 350 °C respectively. Microstructural, phase and mechanical properties analyses were performed following American standard of testing and measurement. The results show that magnesium has influence on the mechanical properties of zinc. The compressive strength, hardness and elastic modulus of 210 ± 8.878 MPa, 76 ± 5.707 HV and 45 ± 11.616 GPa respectively as obtained in Zn-2Mg alloy were optimum and meet the minimum requirement of biodegradable metal for orthopaedics application. These results indicate an increase of 111, 93 and 93% in compressive strength, hardness and elastic modulus respectively as compared to pure zinc. The increase in mechanical properties was adduced to effectiveness of compaction pressure and intermetallic phase formation within the matrix resulting in high dislocation density for improving strength. The study concluded that, Zn-2Mg alloy with optimum mechanical properties can therefore be considered a potential candidate for orthopaedic application.

Keywords: Biodegradable metal, Biomedical application, Mechanical properties, Powder Metallurgy, Zinc

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418 Treatment and Conservation of an Antique Stone Stela by Nano Calcium Hydroxide with Nano Silica in Egyptian Museum of Cairo

Authors: Elhussein Ahmed Elsayed

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An ancient limestone stela dating back to the epoch of the middle kingdom and displayed in the exhibition hall of the middle kingdom, it was discovered in Lisht in Giza, registered with No. 3045 and as a result of its display in an inappropriate display as a result of the use of natural lighting in the display, Represented in sunlight through windows opened day and night. The alternation of these daily changes between the temperature degrees of night and day, both daily and seasonally, causes the expansion and contraction of the rocks and then weakens their cohesion, causing fragmentation. This is indeed the current situation of this stela displayed in the hall, in addition to the damage and fading of colors, as well as the use of a high-viscosity restoration material in the consolidation that led to the attraction of dust and dirt and its adhesion to the surface. The color faded as a result of the lack of lighting control inside the exhibition hall, the remnants of the existing colors were blurred as a result of applying a consolidation material with a high viscosity, which led to the attraction of dust and dirt, and then blurring the colors on the inscription. Examinations and analyzes were carried out on the block, and the results of the examination with a polarized microscope showed that it is of primitive limestone, which contains fossils and microorganisms, which helps to damage. The analysis using the Raman device also showed that the high-viscosity material used in restoration in the past is Paralloid B72. The stone stela was consolidated by using two materials; Nano calcium hydroxide with Nano silica in the form of (Core-shell) at a concentration of 10% and it was applied using the brush.

Keywords: Egyptian museum, stone stela, treatment, nano materials, nano silica

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417 Development and Characterization of a Film Based on Hydroxypropyl Methyl Cellulose Incorporated by a Phenolic Extract of Fennel and Reinforced by Magnesium Oxide: In Vivo - in Vitro

Authors: Mazouzi Nourdjihane, K. Boutemak, A. Haddad, Y. Chegreouche

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In the last decades, biodegradable polymers have been considered as one of the most popular options for the delivery of drugs and various conventional doses. The film forming system (FFS) can be used in topical, transdermal, ophthalmic, oral and gastric applications. Recently this system has focused on improving drug delivery, which can promote drug release. In this context, the aim of this study is to create polymeric film-forming systems for the stomach and to evaluate and test their gastroprotective effects, comparing the effects of changes in composition on film characteristics. It uses a plant-derived polyphenol extract extracted from fennel to demonstrate anti-inflammatory activity in the film. The films are made from hydroxypropyl methylcellulose polymer and different types of plastic, glycerol and polyethylene glycol. The ffs properties show that MgO-glycerol-reinforced hydroxypropylmethylcellulose (HPMC-MgO-Gly) is better than that based on MgO-PEG-reinforced hydroxypropylmethylcellulose (HPMC-MgO-PEG). It is durable, has a faster drying time and allows for maximum recovery. Water vapor strength and blowing speed and other additions show another advantage of HPMC-MgO-Gly compared to HPMC-MgO-PEG, indicating good adhesion between the support (top) and film production. In this study, the gastroprotective effect of fennel phenol extract was found, showing that this plant material has a gastroprotective effect on ulcers and that the film can absorb the active substance.

Keywords: film formin system, hydroxypropyl methylcellulose, magnesium oxide, in vivo

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416 Phyto-Assisted Synthesis of Magnesium Oxide Nanoparticles: Characterization and Applications

Authors: Surendra Kumar Gautam, Mahesh Dhungana

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Magnesium oxide nanoparticles (MgO NPs) are less toxic to humans and the environment as compared to other metal oxide nanoparticles. Various conventional chemical and physical methods are used for synthesis whose toxicity level is high and highly expensive. As the best alternative, phyto-assisted synthesis has emerged, which uses extracts from plant parts for the synthesis of nanoparticles. Here, we report the synthesis of MgO nanoparticles with the assistance of beetroot extract and leaf extract of P. guajava and A. adenophora. The synthesized MgO NPs were characterized by X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), and UV-visible spectroscopy. X-ray analysis for the broadening of peaks was used to evaluate the crystallite size and lattice strain using Debye-Scherer and Williamson–Hall method. The results of crystallite size obtained by both methods are in close proximity. The crystallite size obtained by the Williamson-Hall method seems more accurate, with values being 8.1 nm and 13.2 nm for beetroot MgO NPs and P. guajava MgO NPs, respectively. The FT-IR spectroscopy revealed the dominance of chemical bonds as well as functional groups on MgO NPs surfaces. The UV-visible absorption spectra of MgO NPs were found to be 310 nm, 315 nm, and 315 nm for beetroot, P. guajava, and A. adenophora leaf extract, respectively. Among the three samples, beetroot-mediated MgO NPs were effective antibacterial against both gram-positive and Gram-negative bacteria. In addition, synthesized MgO NPs also show significant antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl radical. Further, beetroot MgO NPs showed the highest photocatalytic activity of about 91% in comparison with other samples.

Keywords: MgO NPs, XRD, FTIR, antibacterial, antioxidant and photocatalytic activity

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415 Obtaining Bioactive Mg-hydroxyapatite Composite Ceramics From Phosphate Rock For Medical Applications

Authors: Sara Mercedes Barroso Pinzón, Antonio Javier Sanchéz Herencia, Begoña Ferrari, Álvaro Jesús Castro

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The current need for durable implants and bone substitutes characterised by biocompatibility, bioactivity and mechanical properties, without immunological rejection, is a major challenge for scientists. Hydroxyapatite (HAp) 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 gives it very low mechanical and biological properties. In this sense, the objective of the research is to address the synthesis of hydroxyapatite with Mg from phosphate rock from sedimentary deposits in the central-eastern region of Colombia, taking advantage of the release of the species contained as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with mineralogical species of 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); as well as the evaluation of the surface physicochemical properties of zeta potential (PZC), with the aim of studying the surface behaviour of the microconstituents present in the phosphate rock and to elucidate the synergistic mechanism between the minerals and establish the optimum conditions for 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 the morphometric parameters, mechanical and biological properties of the designed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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414 Factors Contributing to Adverse Maternal and Fetal Outcome in Patients with Eclampsia

Authors: T. Pradhan, P. Rijal, M. C. Regmi

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Background: Eclampsia is a multisystem disorder that involves vital organs and failure of these may lead to deterioration of maternal condition and hypoxia and acidosis of fetus resulting in high maternal and perinatal mortality and morbidity. Thus, evaluation of the contributing factors for this condition and its complications leading to maternal deaths should be the priority. Formulating the plan and protocol to decrease these losses should be our goal. Aims and Objectives: To evaluate the risk factors associated with adverse maternal and fetal outcome in patients with eclampsia and to correlate the risk factors associated with maternal and fetal morbidity and mortality. Methods: All patients with eclampsia admitted in Department of Obstetrics and Gynecology, B. P. Koirala Institute of Health Sciences were enrolled after informed consent from February 2013 to February 2014. Questions as per per-forma were asked to patients, and attendants like Antenatal clinic visits, parity, number of episodes of seizures, duration from onset of seizure to magnesium sulfate and the patients were followed as per the hospital protocol, the mode of delivery, outcome of baby, post partum maternal condition like maternal Intensive Care Unit admission, neurological impairment and mortality were noted before discharge. Statistical analysis was done using Statistical Package for the Social Sciences (SPSS 11). Mean and percentage were calculated for demographic variables. Pearson’s correlation test and chi-square test were applied to find the relation between the risk factors and the outcomes. P value less than 0.05 was considered significant. Results: There were 10,000 antenatal deliveries during the study period. Fifty-two patients with eclampsia were admitted. All of the patients were unbooked for our institute. Thirty-nine patients were antepartum eclampsia. Thirty-one patients required mechanical ventilator support. Twenty-four patients were delivered by emergency c-section and 21 babies were Low Birth Weight and there were 9 stillbirths. There was one maternal mortality and 45 patients were discharged with improvement but 3 patients had neurological impairment. Mortality was significantly related with number of seizure episodes and time interval between seizure onset and administration of magnesium sulphate. Conclusion: Early detection and management of hypertensive complicating pregnancy during antenatal clinic check up. Early hospitalization and management with magnesium sulphate for eclampsia can help to minimize the maternal and fetal adverse outcomes.

Keywords: eclampsia, maternal mortality, perinatal mortality, risk factors

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413 Study on Temperature Distribution throughout the Continuous Casting Process of Copper Magnesium Alloys

Authors: Paweł Strzępek, Małgorzata Zasadzińska, Szymon Kordaszewski, Wojciech Ściężor

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The constant tendency toward the materials properties improvement nowadays creates opportunities for the scientists, and furthermore the manufacturers all over the world to design, form and produce new alloys almost every day. Considering the fact that companies all over the world look for alloys with the highest values of mechanical properties coexisting with a reasonable electrical conductivity made it necessary to develop new materials based on copper, such as copper magnesium alloys with over 2 wt. % of Mg. Though, before such new material may be mass produced it must undergo a series of tests in order to determine the production technology and its parameters. The presented study is based on the numerical simulations calculated with the use of finite element method analysis, where the geometry of the cooling system, the material used to produce the cooling system and the surface quality of the graphite crystallizer at the place of contact with the cooling system and its influence on the temperatures throughout the continuous casting process is being investigated. The calculated simulations made it possible to propose the optimal set of equipment necessary for the continuous casting process to be carried out in laboratory conditions with various casting parameters and to determine basic materials properties of the obtained alloys such as hardness, electrical conductivity and homogeneity of the chemical composition. The authors are grateful for the financial support provided by The National Centre for Research and Development – Research Project No. LIDER/33/0121/L-11/19/NCBR/2020.

Keywords: CuMg alloys, continuous casting, temperature analysis, finite element method

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412 Effect of Sodium Hydroxide Treatment on the Mechanical Properties of Crushed and Uncrushed Luffa cylindrica Fibre Reinforced rLDPE Composites

Authors: Paschal A. Ubi, Salawu Abdul Rahman Asipita

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The use of suitable engineering materials which poses less harm to ,an and the environment is sort for in recent times, thus giving rise to polymer composites filled with natural organic reinforcement which are biodegradable. Treatment of natural fibres is essential in improving matrix to filler adhesion, hence improving its mechanical properties. In this study, investigations were carried out to determine the effect of sodium hydroxide treatment on the tensile, flexural, impact and hardness properties of crushed and uncrushed luffa cylindrica fibre reinforced recycled low density polyethylene composites. The LC (Luffa Cylindrica) fibres were treated with 0%, 2%, 4%, 6%, 8%, and 10% wt. NaOH concentrations for a period of 24 hours under room temperature conditions. The compounding of the waste LDPE was done using a two roll mill at a temperature of 150 oC and cured in a hydraulic press at a temperature of 150oC for 3 minutes at 3 metric tonnes. A formulation of 20/80g (reinforcement to matrix ratio in grams) was maintained for all fabricated samples. Analysis of the results showed that the uncrushed luffa fibre samples gave better mechanical properties compared with the crushed luffa fibre samples. The uncrushed luffa fibre composites had optimum tensile and flexural strengths of 7.65MPa and 17.08Mpa respectively corresponding to a young modulus and flexural modulus of 21.08MPa and 232.22MPa for the 8% and 4%wt. NaOH concentration respectively. Results obtained in the research showed that NaOH treatment with the 8% NaOH concentration improves the mechanical properties of the LC fibre reinforced composites when compared with other NaOH treatment concentration values.

Keywords: LC fibres, NaOH concentration, LC/rLDPE composite, tensile strength, flexural strength

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411 Identifying Controlling Factors for the Evolution of Shallow Groundwater Chemistry of Ellala Catchment, Northern Ethiopia

Authors: Grmay Kassa Brhane, Hailemariam Siyum Mekonen

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This study was designed to identify the hydrogeochemical and anthropogenic processes controlling the evaluation of groundwater chemistry in the Ellala catchment which covers about 296.5 km2 areal extent. The chemical analysis revealed that the major ions in the groundwater are Ca2+, Mg2+, Na+, and K+ (cations) and HCO3-, PO43-, Cl-, NO3-, and SO42-(anions). Most of the groundwater samples (68.42%) revealed that the groundwater in the catchment is non-alkaline. In addition to the contribution of aquifer material, the solid materials and liquid wastes discharged from different sources can be the main sources of pH and EC in the groundwater. It is observed that the EC of the groundwater is fairly correlated with the DTS. This indicates that high mineralized water is more conductor than water with low concentration. The degree of salinity of the groundwater increases along the groundwater flow path from East to West; then, areas surrounding Mekelle City are highly saline due to the liquid and solid wastes discharged from the city and the industries. The groundwater facies in the catchment are predominated with calcium, magnesium, and bicarbonate which are labeled as Ca-Mg-HCO3 and Mg-Ca-HCO3. The main geochemical process controlling the evolution of the groundwater chemistry in the catchment is rock-water interaction, particularly carbonate dissolution. Due to the clay layer in the aquifer, the reverse is ion exchange. Non-significant silicate weathering and halite dissolution also contribute to the evolution of groundwater chemistry in the catchment. The groundwater in the catchment is dominated by the meteoritic origin although it needs further groundwater chemistry study with isotope dating analysis. The groundwater is under-saturated with calcite, dolomite, and aragonite minerals; hence, the more these minerals encounter the groundwater, the more the minerals dissolve. The main source of calcium and magnesium in groundwater is the dissolution of carbonate minerals (calcite and dolomite) since carbonate rocks are the dominant aquifer materials in the catchment. In addition to this, the weathering of dolerite rock is a possible source of magnesium ions. The relatively higher concentration of sodium over chloride indicates that the source of sodium-ion is reverse ion exchange and/or weathering of sodium-bearing materials, such as shale and dolerite rather than halite dissolution. High concentration of phosphate, nitrate, and chloride in the groundwater is the main anthropogenic source that needs treatment, quality control, and management in the catchment. From the Base Exchange Index Analysis, it is possible to understand that, in the catchment, the groundwater is dominated by the meteoritic origin, although it needs further groundwater chemistry study with isotope dating analysis.

Keywords: Ellala catchment, factor, chemistry, geochemical, groundwater

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410 Ecological Studies on Bulinus truncatus Snail the Intermediate Host of Schistosoma haematobium, in White Nile State, Sudan

Authors: Mohammed Hussein Eltoum Salih

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This study was conducted in four villages, namely: Jadeed, Alandraba, Um Gaar, and EL Shetabe in the White Nile State Sudan, to determine the ecological factors; water vegetations, physical and chemical properties of the water in Snails habitat. Bulinus truncatus, which act as an intermediate host for S. haematobium, were collected from water bodies adjacent to study villages where the residents were suspected to swim, and humans get in contact with water for various purposes. Water samples from the stretches were collected and then measured for parameters that are indicative of the quality of water and sustaining the survival of snails and would confirm even further if the contact between humans and water had taken place. The parameters measured included water conductivity, pH, dissolved oxygen, calcium, and magnesium content. Also, a single water sample from each contact site was collected for microbiological tests. The result revealed that the B. truncatus showed that these animals were fewer and free of infection and their sites of the collection were dense with different plant species making them suitable to harbor snails. Moreover, the results of microbial tests showed that there was higher bacterial contamination. Also, physical and chemical analysis of water sample of contact sites revealed that there were significant differences (p < 0.05) in water pH, calcium, and magnesium content between sites of study villages, and these were discussed in relation to factors suitable for the intermediate hosts and thus for the transmission of the S. haematobium disease.

Keywords: health, parasitology, Schistosoma, snails

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409 Improving Biodegradation Behavior of Fabricated WE43 Magnesium Alloy by High-Temperature Oxidation

Authors: Jinge Liu, Shuyuan Min, Bingchuan Liu, Bangzhao Yin, Bo Peng, Peng Wen, Yun Tian

Abstract:

WE43 magnesium alloy can be additively manufactured via laser powder bed fusion (LPBF) for biodegradable applications, but the as-built WE43 exhibits an excessively rapid corrosion rate. High-temperature oxidation (HTO) was performed on the as-built WE43 to improve its biodegradation behavior. A sandwich structure including an oxide layer at the surface, a transition layer in the middle, and the matrix was generated influenced by the oxidation reaction and diffusion of RE atoms when heated at 525 ℃for 8 hours. The oxide layer consisted of Y₂O₃ and Nd₂O₃ oxides with a thickness of 2-3 μm. The transition layer is composed of α-Mg and Y₂O₃ with a thickness of 60-70 μm, while Mg24RE5 could be observed except α-Mg and Y₂O₃. The oxide layer and transition layer appeared to have an effective passivation effect. The as-built WE43 lost 40% weight after the in vitro immersion test for three days and finally broke into debris after seven days of immersion. The high-temperature oxidation samples kept the structural integrity and lost only 6.88 % weight after 28-day immersion. The corrosion rate of HTO samples was significantly controlled, which improved the biocompatibility of the as-built WE43 at the same time. The samples after HTO had better osteogenic capability according to ALP activity. Moreover, as built WE43 performed unqualified in cell adhesion and hemolytic test due to its excessively rapid corrosion rate. While as for HTO samples, cells adhered well, and the hemolysis ratio was only 1.59%.

Keywords: laser powder bed fusion, biodegradable metal, high temperature oxidation, biodegradation behavior, WE43

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408 Positive effect of Cu2+ and Ca2+ on the Thermostability of Bambara Groundnut Peroxidase A6, and its Catalytic Efficiency Toward the Oxidation of 3,3,5,5 -Tetramethyl Benzidine

Authors: Yves Mann Elate Lea Mbassi, Marie Solange Evehe Bebandoue, Wilfred Fon Mbacham

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Improving the catalytic performance of enzymes has been a long-standing theme of analytical biochemistry research. Induction of peroxidase activity by metals is a common reaction in higher plants. We thought that this increase in peroxidase activity may be due, on the one hand, to the stimulation of the gene expression of these enzymes but also to a modification of their chemical reactivity following the binding of some metal ions on their active site. We tested the effect of some metal salts (MgCl₂, MnCl₂, ZnCl₂, CaCl₂ and CuSO₄) on the activity and thermostability of peroxidase A6, a thermostable peroxidase that we discovered and purified in a previous study. The chromogenic substrate used was 3,3′,5,5′-tetramethylbenzidine. Of all the metals tested for their effect on A6, only magnesium and copper had a significant effect on the activity of the enzyme at room temperature. The Mann-Whitney test shows a slight inhibitory effect of activity by the magnesium salt (P = 0.043), while the activity of the enzyme is 5 times higher in the presence of the copper salt (P = 0.002). Moreover, the thermostability of peroxidase A6 is increased when calcium and copper salts are present. The activity in the presence of CaCl₂ is 8 times higher than the residual activity of the enzyme alone after incubation at 80°C for 10 min and 35 times higher in the presence of CuSO4 under the same conditions. In addition, manganese and zinc salts slightly reduce the thermostability of the enzyme. The activity and structural stability of peroxidase A6 can clearly be activated by Cu₂+, which therefore enhance the oxidation of 3,3′,5,5′-tetramethylbenzidine, which was used in this study as a chromogenic substrate. Ca₂+ likely has a more stabilizing function for the catalytic site.

Keywords: peroxidase activity, copper ions, calcium ions, thermostability

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407 The Effects of Wood Ash on Ignition Point of Wood

Authors: K. A. Ibe, J. I. Mbonu, G. K. Umukoro

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The effects of wood ash on the ignition point of five common tropical woods in Nigeria were investigated. The ash and moisture contents of the wood saw dust from Mahogany (Khaya ivorensis), Opepe (Sarcocephalus latifolius), Abura (Hallealedermannii verdc), Rubber (Heavea brasilensis) and Poroporo (Sorghum bicolour) were determined using a furnace (Vecstar furnaces, model ECF2, serial no. f3077) and oven (Genlab laboratory oven, model MINO/040) respectively. The metal contents of the five wood sawdust ash samples were determined using a Perkin Elmer optima 3000 dv atomic absorption spectrometer while the ignition points were determined using Vecstar furnaces model ECF2. Poroporo had the highest ash content, 2.263 g while rubber had the least, 0.710 g. The results for the moisture content range from 2.971 g to 0.903 g. Magnesium metal had the highest concentration of all the metals, in all the wood ash samples; with mahogany ash having the highest concentration, 9.196 ppm while rubber ash had the least concentration of magnesium metal, 2.196 ppm. The ignition point results showed that the wood ashes from mahogany and opepe increased the ignition points of the test wood samples when coated on them while the ashes from poroporo, rubber and abura decreased the ignition points of the test wood samples when coated on them. However, Opepe saw dust ash decreased the ignition point in one of the test wood samples, suggesting that the metal content of the test wood sample was more than that of the Opepe saw dust ash. Therefore, Mahogany and Opepe saw dust ashes could be used in the surface treatment of wood to enhance their fire resistance or retardancy. However, the caution to be exercised in this application is that the metal content of the test wood samples should be evaluated as well.

Keywords: ash, fire, ignition point, retardant, wood saw dust

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406 An Acyclic Zincgermylene: Rapid H₂ Activation

Authors: Martin Juckel

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Probably no other field of inorganic chemistry has undergone such a rapid development in the past two decades than the low oxidation state chemistry of main group elements. This rapid development has only been possible by the development of new bulky ligands. In case of our research group, super-bulky monodentate amido ligands and β-diketiminate ligands have been used to a great success. We first synthesized the unprecedented magnesium(I) dimer [ᴹᵉˢNacnacMg]₂ (ᴹᵉˢNacnac = [(ᴹᵉˢNCMe)₂CH]-; Mes = mesityl, which has since been used both as reducing agent and also for the synthesis of new metal-magnesium bonds. In case of the zinc bromide precursor [L*ZnBr] (L*=(N(Ar*)(SiPri₃); (Ar* = C₆H₂{C(H)Ph₂}₂Me-2,6,4, the reduction with [ᴹᵉˢNacnacMg]₂ led to such a metal-magnesium bond. This [L*ZnMg(ᴹᵉˢNacnac)] compound can be seen as an ‘inorganic Grignard reagent’, which can be used to transfer the metal fragment onto other functional groups or other metal centers; just like the conventional Grignard reagent. By simple addition of (TBoN)GeCl (TBoN = N(SiMe₃){B(DipNCH)₂) to the aforesaid compound, we were able to transfer the amido-zinc fragment to the Ge center of the germylene starting material and to synthesize the first example of a germanium(II)-zinc bond: [:Ge(TBoN)(ZnL*)]. While these reactions typically led to complex product mixture, [:Ge(TBoN)(ZnL*)] could be isolated as dark blue crystals in a good yield. This new compound shows interesting reactivity towards small molecules, especially dihydrogen gas. This is of special interest as dihydrogen is one of the more difficult small molecules to activate, due to its strong (BDE = 108 kcal/mol) and non-polar bond. In this context, the interaction between H₂ σ-bond with the tetrelylene p-Orbital (LUMO), with concomitant donation of the tetrelylene lone pair (HOMO) into the H₂ σ* orbital are responsible for the activation of dihydrogen gas. Accordingly, the narrower the HOMO-LUMO gap of tertelylene, the more reactivity towards H₂ it typically is. The aim of a narrow HOMO-LUMO gap was reached by transferring electropositive substituents respectively metal substituents with relatively low Pauling electronegativity (zinc: 1.65) onto the Ge center (here: the zinc-amido fragment). In consideration of the unprecedented reactivity of [:Ge(TBoN)(ZnL*)], a computational examination of its frontier orbital energies was undertaken. The energy separation between the HOMO, which has significant Ge lone pair character, and the LUMO, which has predominantly Ge p-orbital character, is narrow (40.8 kcal/mol; cf.∆S-T= 24.8 kcal/mol), and comparable to the HOMO-LUMO gaps calculated for other literature known complexes). The calculated very narrow HOMO-LUMO gap for the [:Ge(TBoN)(ZnL*)] complex is consistent with its high reactivity, and is remarkable considering that it incorporates a π-basic amide ligand, which are known to raise the LUMO of germylenes considerably.

Keywords: activation of dihydrogen gas, narrow HOMO-LUMO gap, first germanium(II)-zinc bond, inorganic Grignard reagent

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