Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 8431

Search results for: solid state synthesis

8431 Reference Intensity Ratio Semi-Quantitative Analysis of Cordierite-Mullite Synthesis by a Solid State Method

Authors: D. Wattanasiriwech, S. Wattanasiriwech


In this paper, attempt to synthesize designed cordierite-mullite system with various ratios was performed using a solid-state method. Alumina, quartz, magnesia, and talc were used as starting materials for the synthesis. Talc was added for two purposes; to assist the reaction progress and to be the Mg source. The raw materials were mixed and fired at 1350°C for 2 h and 1400°C for 2 and 4 h. The resulting phase compositions were analysed using the Reference Intensity Ratio (RIR) semi-quantitative analysis method. The highest amount of cordierite up to Cordierite phase 96% could be obtained at the firing scheme of 1400°C for 4 h in the C100-M0. Mullite could not be formed at the selected scheme if talc did not present so no pure mullite was observed in the selected firing regime. The highest amount of mullite co-existed with cordierite and other phases were 74%.

Keywords: RIR semi-quantitative analysis, cordierite-mullite system, solid state synthesis, X-Ray diffraction

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8430 Synthesis, Characterization and Electrical Studies of Solid Polymer Electrolyte (1-x) PANI-KAg₄I₅.xAl₂O₃

Authors: Rafiuddin


Solid polymer electrolytes have emerged as an area of interest in the field of solid state chemistry owing to their facile and cost-effective synthesis and number of applications in different areas of chemistry, extending over a wide range of temperatures. In the present work, polymer composite solid electrolyte comprising of Polyaniline (PANI) as polymer and potassium silver iodide (KAg4I5) using alumina (Al2O3) of different compositions having the formula (1-x) PANI- KAg4I5. x Al2O3 with x ranging from 0.0 to 0.5 was prepared by solid state reaction method. The structural elucidation and characterization was done by X- Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric- Differential Thermal Analysis (TG-DTA) and Impedance Spectroscopy. The thermal analysis shows a phase transition at 147°C attributed to β-α phase transition of AgI due to the disproportionation of KAg4I5 to AgI and KAg2I3 at temperatures higher than 36°C. The X Ray diffraction analysis also confirms the presence of both AgI and KAg2I3 in the samples. The conductivities recorded over a temperature range of 40-250° C lie in the range of 10-1 to 10-3 S cm-1. Maximum conductivity was seen in the compositon x = 0.4 i.e. 1.84 × 10-2 Scm-1 at 313 K and 1.38 × 10-1 Scm-1 at 513 K, with a minimum activation energy of 0.14 eV.

Keywords: polymer solid electrolytes, XRD, DTA, electrical conductivity, impedance spectroscopy

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8429 Effect of Iron Oxide Addition on the Solid-State Synthesis of Ye’Elimite

Authors: F. Z. Abir, M. Mesnaoui, Y. Abouliatim, L. Nibou, Y. El Hafiane, A. Smith


The cement industry has been taking significant steps for years to reduce its carbon footprint by opting for an eco-friendly alternative such as Calcium Sulfoaluminate Cements (CSA). These binders, compared to Ordinary Portland Cements (OPC), have two advantages: reduction of the CO2 emissions and energy-saving because the sintering temperature of CSA cements is between 1250 and 1350 °C, which means 100 to 200 °C less than OPC. The aim of this work is to study the impurities effect, such as iron oxide, on the formation of the ye'elimite phase, which represents the main phase of Calcium Sulfoaluminate Cements and the consequence on its hydration. Several elaborations and characterization techniques were used to study the structure and microstructure of ye'elimite, such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), thermal analysis, specific surface area measurement, and electrical conductivity of diluted solutions. This study details the protocol for the solid-state synthesis of ye'elimite containing increasing amounts of iron (general formula: Ca4Al(6-2x)Fe2xSO16 with x = 0.00 to 1.13). Ye'elimite is formed by solid-state reactions between Al2O3, CaO and CaSO4 and the maximum ye'elimite content is reached at a sintering temperature of 1300 °C. The presence of iron promotes the formation of cubic ye'elimite at the expense of the orthorhombic phase. The total incorporation of iron in ye'elimite structure is possible when x < 0.12. Beyond this content, the ferritic phase (CaO)2(Al2O3,Fe2O3) appears as a minor phase and develops two different morphologies during cooling: dendritic crystals and melt morphology. The formation of the ferrous liquid phase affects the evolution of grain size of the ye’elimite and calcium aluminates.

Keywords: calcium sulfoaluminate cement, ferritic phase, sintering, solid-state synthesis, ye’elimite

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8428 Synthesis of a Serie of Metallic Complexes Derived from bis(4-Amino-5-Mercapto-1,2,4-Triazol-3-yl)butane with First Raw Transition Metals

Authors: I. Belbachir, T. Benabdallah, N. Belhadj


The present research work describes the synthesis, through a multi-step strategy, as well as the structural characterization of a polydentate organic ligand, namely the bis(4-amino-5-mercapto-1,2,4-triazole-3-yl)butane (BAMT). The bis-triazolic ligand was characterized by different spectroscopic studies, in order to enlighten its coordination mode, in the neutral and deprotonated forms, towards cobalt(II), nickel(II) and copper(II) sulfates, in both solution and solid state. The stoichiometry of the complexes [neutral BAMT-metal] and [deprotonated BAMT-metal] was first established in a solution of DMF with each of the three metallic cations and their complexation constants calculated, allowing us to compare the stability of the various prepared complexes. The various complexes were finally isolated in the solid state and the coordination mode of neutral and deprotonated BAMT explored towards each of the three metallic sulfates. The establishment of some ligand field parameters (Dq, B, β…) by electronic spectroscopy finally allowed to compare the coordination modes of BAMT towards each of the three metals and to highlight the influence of the deprotonation on the complexing properties of the bis-triazolic ligand.

Keywords: 1, 2, 4-triazol, bis-1, 2, 4-triazol, metallic complexes, coordination in solution and solid state

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8427 Definition of Service Angle of Android’S Robot Hand by Method of Small Movements of Gripper’S Axis Synthesis by Speed Vector

Authors: Valeriy Nebritov


The paper presents a generalized method for determining the service solid angle based on the assigned gripper axis orientation with a stationary grip center. Motion synthesis in this work is carried out in the vector of velocities. As an example, a solid angle of the android robot arm is determined, this angle being formed by the longitudinal axis of a gripper. The nature of the method is based on the study of sets of configuration positions, defining the end point positions of the unit radius sphere sweep, which specifies the service solid angle. From this the spherical curve specifying the shape of the desired solid angle was determined. The results of the research can be used in the development of control systems of autonomous android robots.

Keywords: android robot, control systems, motion synthesis, service angle

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8426 Co-Synthesis of Exopolysaccharides and Polyhydroxyalkanoates Using Waste Streams: Solid-State Fermentation as an Alternative Approach

Authors: Laura Mejias, Sandra Monteagudo, Oscar Martinez-Avila, Sergio Ponsa


Bioplastics are gaining attention as potential substitutes of conventional fossil-derived plastics and new components of specialized applications in different industries. Besides, these constitute a sustainable alternative since they are biodegradable and can be obtained starting from renewable sources. Thus, agro-industrial wastes appear as potential substrates for bioplastics production using microorganisms, considering they are a suitable source for nutrients, low-cost, and available worldwide. Therefore, this approach contributes to the biorefinery and circular economy paradigm. The present study assesses the solid-state fermentation (SSF) technology for the co-synthesis of exopolysaccharides (EPS) and polyhydroxyalkanoates (PHA), two attractive biodegradable bioplastics, using the leftover of the brewery industry brewer's spent grain (BSG). After an initial screening of diverse PHA-producer bacteria, it was found that Burkholderia cepacia presented the highest EPS and PHA production potential via SSF of BSG. Thus, B. cepacia served to identify the most relevant aspects affecting the EPS+PHA co-synthesis at a lab-scale (100g). Since these are growth-dependent processes, they were monitored online through oxygen consumption using a dynamic respirometric system, but also quantifying the biomass production (gravimetric) and the obtained products (EtOH precipitation for EPS and solid-liquid extraction coupled with GC-FID for PHA). Results showed that B. cepacia has grown up to 81 mg per gram of dry BSG (gDM) at 30°C after 96 h, representing up to 618 times higher than the other tested strains' findings. Hence, the crude EPS production was 53 mg g-1DM (2% carbohydrates), but purity reached 98% after a dialysis purification step. Simultaneously, B. cepacia accumulated up to 36% (dry basis) of the produced biomass as PHA, mainly composed of polyhydroxybutyrate (P3HB). The maximum PHA production was reached after 48 h with 12.1 mg g⁻¹DM, representing threefold the levels previously reported using SSF. Moisture content and aeration strategy resulted in the most significant variables affecting the simultaneous production. Results show the potential of co-synthesis via SSF as an attractive alternative to enhance bioprocess feasibility for obtaining these bioplastics in residue-based systems.

Keywords: bioplastics, brewer’s spent grain, circular economy, solid-state fermentation, waste to product

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8425 Fast High Voltage Solid State Switch Using Insulated Gate Bipolar Transistor for Discharge-Pumped Lasers

Authors: Nur Syarafina Binti Othman, Tsubasa Jindo, Makato Yamada, Miho Tsuyama, Hitoshi Nakano


A novel method to produce a fast high voltage solid states switch using Insulated Gate Bipolar Transistors (IGBTs) is presented for discharge-pumped gas lasers. The IGBTs are connected in series to achieve a high voltage rating. An avalanche transistor is used as the gate driver. The fast pulse generated by the avalanche transistor quickly charges the large input capacitance of the IGBT, resulting in a switch out of a fast high-voltage pulse. The switching characteristic of fast-high voltage solid state switch has been estimated in the multi-stage series-connected IGBT with the applied voltage of several tens of kV. Electrical circuit diagram and the mythology of fast-high voltage solid state switch as well as experimental results obtained are presented.

Keywords: high voltage, IGBT, solid state switch, bipolar transistor

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8424 Synthesis, Microstructure and Photoluminescence Properties of Yttrium Orthovanadates: Influences of Silica Nano-Particles and Nano-Layers

Authors: Seyed Mahdi Rafiaei


In this investigation, firstly Eu3+ doped YVO4 phosphor was synthesized using solid-state method. Then silica was coated on the surface of particles via sol-gel method. To study the influence of SiO2 addition on microstructure and photoluminescence characteristics of YVO4:4% Eu3+ phosphor materials, we employed X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High-Resolution Transmitted Electron Microscope (HRTEM), Focused Ion Beam (FIB), Brunauer Emmett Teller (BET), Inductively coupled plasma (ICP), Electron Spin Resonance (ESR) and Photoluminescence (PL) equipments. The XPS characterization confirmed the formation of Y–O–Si and V-O-Si bondings between YVO4:Eu3+ phosphor particle and SiO2 coating. In addition, it was found that although the amounts of added SiO2 were not remarkable, but it resulted in enhancement of emission intensity of the phosphors. Finally by employing ESR analysis, it was shown that surface oxygen vacancies, result in reduction of V5+ to the lower valence state of V4+.

Keywords: solid state, sol-gel, silica, coating, photoluminescence

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8423 Structural Investigation and Hyperfine Interactions of BaBiₓLaₓFe₁₂₋₂ₓO₁₉ (0.0 ≤ X ≤ 0.5) Hexaferrites

Authors: Hakan Gungunes, Ismail A. Auwal, Abdulhadi Baykal, Sagar E. Shirsath


Barium hexaferrite, BaFe₁₂O₁₉, substituted by Bi³⁺ and La³⁺ (BaBiₓLaₓFe₁₂₋₂ₓO₁₉ where 0.0 ≤ x ≤ 0.5) were prepared by solid state synthesis route. The effect of substituted Bi³⁺ and La³⁺ ions on the structure, morphology, magnetic and cation distributions of barium hexaferrite were investigated by X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR) and Mössbauer spectroscopy. XRD powder patterns were refined by the Rietveld analysis method which confirmed the formation of single phase magneto-plumbite structure and the substitution of La³⁺ and Bi³⁺ ions into the lattice of barium ferrite. These results show that both La³⁺ and Bi³⁺ ions completely enter into barium hexaferrite lattice without disturbing the hexagonal ferrite structure. The EDX spectra confirmed the presence of all the constituents in expected elemental percentage. From 57Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values on Bi and La substitutions have been determined. Cation distribution in the presently investigated hexaferrite system was estimated using the relative area of Mössbauer spectroscopy.

Keywords: hexaferrite, mössbauer, cation distribution, solid state synthesis

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8422 Total Synthesis of Natural Cyclic Depsi Peptides by Convergent SPPS and Macrolactonization Strategy for Anti-Tb Activity

Authors: Katharigatta N. Venugopala, Fernando Albericio, Bander E. Al-Dhubiab, T. Govender


Recent years have witnessed a renaissance in the field of peptides that are obtained from various natural sources such as many bacteria, fungi, plants, seaweeds, vertebrates, invertebrates and have been reported for various pharmacological properties such as anti-TB, anticancer, antimalarial, anti-inflammatory, anti-HIV, antibacterial, antifungal, and antidiabetic, activities. In view of the pharmacological significance of natural peptides, serious research efforts of many scientific groups and pharmaceutical companies have consequently focused on them to explore the possibility of developing their potential analogues as therapeutic agents. Solid phase and solution phase peptide synthesis are the two methodologies currently available for the synthesis of natural or synthetic linear or cyclic depsi-peptides. From a synthetic point of view, there is no doubt that the solid-phase methodology gained added advantages over solution phase methodology in terms of simplicity, purity of the compound and the speed with which peptides can be synthesised. In the present study total synthesis, purification and structural elucidation of analogues of natural anti-TB cyclic depsi-peptides such as depsidomycin, massetolides and viscosin has been attempted by solid phase method using standard Fmoc protocols and finally off resin cyclization in solution phase method. In case of depsidomycin, synthesis of linear peptide on solid phase could not be achieved because of two turn inducing amino acids in the peptide sequence, but total synthesis was achieved by convergent solid phase peptide synthesis followed by cyclization in solution phase method. The title compounds obtained were in good yields and characterized by NMR and HRMS. Anti-TB results revealed that the potential title compound exhibited promising activity at 4 µg/mL against H37Rv and 16 µg/mL against MDR strains of tuberculosis.

Keywords: total synthesis, cyclic depsi-peptides, anti-TB activity, tuberculosis

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8421 Synthesis and Characterization of Pure and Doped Li7La3Zr2O12 Li-Ion Conducting Solid Electrolyte for Lithium Batteries

Authors: Shari Ann S. Botin, Ruziel Larmae T. Gimpaya, Rembrant Rockwell Gamboa, Rinlee Butch M. Cervera


In recent years, demand for the use of solid electrolytes as alternatives to liquid electrolytes has increased due to recurring battery safety and stability issues, in addition to an increase in energy density requirement which can be made possible by using solid electrolytes. Among the solid electrolyte systems, Li7La3Zr2O12 (LLZ) is one of the most promising as it exhibits good chemical stability against Li metal and has a relatively high ionic conductivity. In this study, pure and doped LLZ were synthesized via conventional solid state reaction. The precursor chemicals (such as LiOH, La2O3, Ga2O3 and ZrO2) were ground and then calcined at 900 °C, pressed into pellets and finally sintered at 1000 °C to 1200 °C. The microstructure and ionic conductivity of the obtained samples have been investigated. Results show that for pure LLZ, sintering at lower temperature (1000 °C) produced tetragonal LLZ while sintering at higher temperatures (≥ 1150 °C) produced cubic LLZ based from the XRD results. However, doping with Ga produces an easier formation of LLZ with cubic structure at lower sintering duration. On the other hand, the lithium conductivity of the samples was investigated using electrochemical impedance spectroscopy at room temperature. Among the obtained samples, Ga-doped LLZ sintered at 1150 °C obtained the highest ionic conductivity reaching to about 1x10⁻⁴ S/cm at room temperature. In addition, fabrication and initial investigation of an all-solid state Lithium Battery using the synthesized LLZ sample with the use of commercial cathode materials have been investigated.

Keywords: doped LLZ, lithium-ion battery, pure LLZ, solid electrolytes

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8420 The Effect of the Precursor Powder Size on the Electrical and Sensor Characteristics of Fully Stabilized Zirconia-Based Solid Electrolytes

Authors: Olga Yu Kurapova, Alexander V. Shorokhov, Vladimir G. Konakov


Nowadays, due to their exceptional anion conductivity at high temperatures cubic zirconia solid solutions, stabilized by rare-earth and alkaline-earth metal oxides, are widely used as a solid electrolyte (SE) materials in different electrochemical devices such as gas sensors, oxygen pumps, solid oxide fuel cells (SOFC), etc. Nowadays the intensive studies are carried out in a field of novel fully stabilized zirconia based SE development. The use of precursor powders for SE manufacturing allows predetermining the microstructure, electrical and sensor characteristics of zirconia based ceramics used as SE. Thus the goal of the present work was the investigation of the effect of precursor powder size on the electrical and sensor characteristics of fully stabilized zirconia-based solid electrolytes with compositions of 0,08Y2O3∙0,92ZrO2 (YSZ), 0,06Ce2O3∙ 0,06Y2O3∙0,88ZrO2 and 0,09Ce2O3∙0,06Y2O3-0,85ZrO2. The synthesis of precursors powders with different mean particle size was performed by sol-gel synthesis in the form of reversed co-precipitation from aqueous solutions. The cakes were washed until the neutral pH and pan-dried at 110 °С. Also, YSZ ceramics was obtained by conventional solid state synthesis including milling into a planetary mill. Then the powder was cold pressed into the pellets with a diameter of 7.2 and ~4 mm thickness at P ~16 kg/cm2 and then hydrostatically pressed. The pellets were annealed at 1600 °С for 2 hours. The phase composition of as-synthesized SE was investigated by X-Ray photoelectron spectroscopy ESCA (spectrometer ESCA-5400, PHI) X-ray diffraction analysis - XRD (Shimadzu XRD-6000). Following galvanic cell О2 (РО2(1)), Pt | SE | Pt, (РО2(2) = 0.21 atm) was used for SE sensor properties investigation. The value of РО2(1) was set by mixing of O2 and N2 in the defined proportions with the accuracy of  5%. The temperature was measured by Pt/Pt-10% Rh thermocouple, The cell electromotive force (EMF) measurement was carried out with ± 0.1 mV accuracy. During the operation at the constant temperature, reproducibility was better than 5 mV. Asymmetric potential measured for all SE appeared to be negligible. It was shown that the resistivity of YSZ ceramics decreases in about two times upon the mean agglomerates decrease from 200-250 to 40 nm. It is likely due to the both surface and bulk resistivity decrease in grains. So the overall decrease of grain size in ceramic SE results in the significant decrease of the total ceramics resistivity allowing sensor operation at lower temperatures. For the SE manufactured the estimation of oxygen ion transfer number tion was carried out in the range 600-800 °С. YSZ ceramics manufactured from powders with the mean particle size 40-140 nm, shows the highest values i.e. 0.97-0.98. SE manufactured from precursors with the mean particle size 40-140 nm shows higher sensor characteristic i.e. temperature and oxygen concentration EMF dependencies, EMF (ENernst - Ereal), tion, response time, then ceramics, manufactured by conventional solid state synthesis.

Keywords: oxygen sensors, precursor powders, sol-gel synthesis, stabilized zirconia ceramics

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8419 The Optimum Operating Conditions for the Synthesis of Zeolite from Waste Incineration Fly Ash by Alkali Fusion and Hydrothermal Methods

Authors: Yi-Jie Lin, Jyh-Cherng Chen


The fly ash of waste incineration processes is usually hazardous and the disposal or reuse of waste incineration fly ash is difficult. In this study, the waste incineration fly ash was converted to useful zeolites by the alkali fusion and hydrothermal synthesis method. The influence of different operating conditions (the ratio of Si/Al, the ratio of hydrolysis liquid to solid, and hydrothermal time) was investigated to seek the optimum operating conditions for the synthesis of zeolite from waste incineration fly ash. The results showed that concentrations of heavy metals in the leachate of Toxicity Characteristic Leaching Procedure (TCLP) were all lower than the regulatory limits except lead. The optimum operating conditions for the synthesis of zeolite from waste incineration fly ash by the alkali fusion and hydrothermal synthesis method were Si/Al=40, NaOH/ash=1.5, alkali fusion at 400 oC for 40 min, hydrolysis with Liquid to Solid ratio (L/S)= 200 at 105 oC for 24 h, and hydrothermal synthesis at 105 oC for 24 h. The specific surface area of fly ash could be significantly increased from 8.59 m2/g to 651.51 m2/g (synthesized zeolite). The influence of different operating conditions on the synthesis of zeolite from waste incineration fly ash followed the sequence of Si/Al ratio > hydrothermal time > hydrolysis L/S ratio. The synthesized zeolites can be reused as good adsorbents to control the air or wastewater pollutants. The purpose of fly ash detoxification, reduction and waste recycling/reuse is achieved successfully.

Keywords: alkali fusion, hydrothermal, fly ash, zeolite

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8418 Synthesis of Solid Polymeric Materials by Maghnite-H⁺ as a Green Catalyst

Authors: Draoua Zohra, Harrane Amine


The Solid Polymeric Materials have been successfully prepared by the copolymerization of e-caprolactone (CL) and poly (ethylene glycol) (PEG) employing Maghnite-H+ at 80°C. Maghnite-H+ is a solid catalyst non-toxic. The presence of PEG chains leads to a break in the growth of PCL chains and consequently leads to the copolymer tri-block PCL-PEG-PCL. The objective of this study was to synthesize and characterize of Solid Polymeric Materials. The highly hydrophilic nature of polyethylene glycol has sparked our interest in developing a Solid Polymeric based e-caprolactone and poly (ethylene glycol). PCL and PEG are biocompatible materials. Their ring-opening copolymerization using Maghnite H+ makes to the Solid Polymeric Materials. The morphology and structure of Solid polymeric Materials were characterized by ¹H and ¹³C-NMR spectra and Gel Permeation Chromatography (GPC). This paper developed the application of Maghnite-H+ as an efficient catalyst by an easy-to-handle procedure to get solid polymeric materials. A cationic mechanism for the copolymerization reaction was proposed.

Keywords: block copolymers, maghnite, montmorillonite, poly(e-caprolactone)

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8417 Friction Stir Welding Process as a Solid State Joining -A Review

Authors: Mohd Anees Siddiqui, S. A. H. Jafri, Shahnawaz Alam


Through this paper an attempt is made to review a special welding technology of friction stir welding (FSW) which is a solid-state joining. Friction stir welding is used for joining of two plates which are applied compressive force by using fixtures over the work table. This is a non consumable type welding technique in which a rotating tool of cylindrical shape is used. Process parameters such as tool geometry, joint design and process speed are discussed in the paper. Comparative study of Friction stir welding with other welding techniques such as MIG, TIG & GMAW is also done. Some light is put on several major applications of friction stir welding in different industries. Quality and environmental aspects of friction stir welding is also discussed.

Keywords: friction stir welding (FSW), process parameters, tool, solid state joining processes

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8416 The Legal Framework for Solid Waste Disposal and Management in Kwara State, Nigeria

Authors: Alabi Odunayo Mayowa, Ajayi Oluwasola Felix


Solid waste such as “garbage” “trash” “refuse” “slug” and “rubbish” is disposed off or is required to be disposed off in accordance with national law. The study relies on primary and secondary sources of information. The primary sources include the Constitution, statutes and subsidiary legislation. The secondary sources of information include books, journals, conference proceedings, newspapers, magazines and internet materials. The information obtained from these sources is subjected to content and contextual analysis. The study examines the Kwara State Environmental Protection Agency Law, 1992 and other laws on waste disposal and management in Kwara State, Nigeria. The study also examines the regulations and the agency i.e. the Kwara State Environmental Protection Agency created by the law with a view to determine the inadequacies in the law.

Keywords: solid waste, waste disposal, waste management, domestic waste

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8415 Speciation Analysis by Solid-Phase Microextraction and Application to Atrazine

Authors: K. Benhabib, X. Pierens, V-D Nguyen, G. Mimanne


The main hypothesis of the dynamics of solid phase microextraction (SPME) is that steady-state mass transfer is respected throughout the SPME extraction process. It considers steady-state diffusion is established in the two phases and fast exchange of the analyte at the solid phase film/water interface. An improved model is proposed in this paper to handle with the situation when the analyte (atrazine) is in contact with colloid suspensions (carboxylate latex in aqueous solution). A mathematical solution is obtained by substituting the diffusion coefficient by the mean of diffusion coefficient between analyte and carboxylate latex, and also thickness layer by the mean thickness in aqueous solution. This solution provides an equation relating the extracted amount of the analyte to the extraction a little more complicated than previous models. It also gives a better description of experimental observations. Moreover, the rate constant of analyte obtained is in satisfactory agreement with that obtained from the initial curve fitting.

Keywords: pesticide, solid-phase microextraction (SPME) methods, steady state, analytical model

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8414 An Impregnated Active Layer Mode of Solution Combustion Synthesis as a Tool for the Solution Combustion Mechanism Investigation

Authors: Zhanna Yermekova, Sergey Roslyakov


Solution combustion synthesis (SCS) is the unique method which multiple times has proved itself as an effective and efficient approach for the versatile synthesis of a variety of materials. It has significant advantages such as relatively simple handling process, high rates of product synthesis, mixing of the precursors on a molecular level, and fabrication of the nanoproducts as a result. Nowadays, an overwhelming majority of solution combustion investigations performed through the volume combustion synthesis (VCS) where the entire liquid precursor is heated until the combustion self-initiates throughout the volume. Less amount of the experiments devoted to the steady-state self-propagating mode of SCS. Under the beforementioned regime, the precursor solution is dried until the gel-like media, and later on, the gel substance is locally ignited. In such a case, a combustion wave propagates in a self-sustaining mode as in conventional solid combustion synthesis. Even less attention is given to the impregnated active layer (IAL) mode of solution combustion. An IAL approach to the synthesis is implying that the solution combustion of the precursors should be initiated on the surface of the third chemical or inside the third substance. This work is aiming to emphasize an underestimated role of the impregnated active layer mode of the solution combustion synthesis for the fundamental studies of the combustion mechanisms. It also serves the purpose of popularizing the technical terms and clarifying the difference between them. In order to do so, the solution combustion synthesis of γ-FeNi (PDF#47-1417) alloy has been accomplished within short (seconds) one-step reaction of metal precursors with hexamethylenetetramine (HTMA) fuel. An idea of the special role of the Ni in a process of alloy formation was suggested and confirmed with the particularly organized set of experiments. The first set of experiments were conducted in a conventional steady-state self-propagating mode of SCS. An alloy was synthesized as a single monophasic product. In two other experiments, the synthesis was divided into two independent processes which are possible under the IAL mode of solution combustion. The sequence of the process was changed according to the equations which are describing an Experiment A and B below: Experiment A: Step 1. Fe(NO₃)₃*9H₂O + HMTA = FeO + gas products; Step 2. FeO + Ni(NO₃)₂*6H₂O + HMTA = Ni + FeO + gas products; Experiment B: Step 1. Ni(NO₃)₂*6H₂O + HMTA = Ni + gas products; Step 2. Ni + Fe(NO₃)₃*9H₂O + HMTA = Fe₃Ni₂+ traces (Ni + FeO). Based on the IAL experiment results, one can see that combustion of the Fe(NO₃)₃9H₂O on the surface of the Ni is leading to the alloy formation while presence of the already formed FeO does not affect the Ni(NO₃)₂*6H₂O + HMTA reaction in any way and Ni is the main product of the synthesis.

Keywords: alloy, hexamethylenetetramine, impregnated active layer mode, mechanism, solution combustion synthesis

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8413 Conventional Synthesis and Characterization of Zirconium Molybdate, Nd2Zr3(MoO4)9

Authors: G. Çelik Gül, F. Kurtuluş


Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd2Zr3(MoO4)9 which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd₂Zr₃(MoO₄)₉, powder x-ray diffraction, solid state synthesis, zirconium molybdates

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8412 Effect of Sintering Temperature on Transport Properties of Garnet-Type Solid-State Electrolytes for Energy Storage Systems

Authors: U. Farooq, A. Samson, V. Thangadurai, R. Edwards


In recent years, an impressive research has been conducted to introduce the solid-state electrolytes for the future energy storage devices like Li-ion batteries more specifically. In this work we tried to prepare a ceramic electrolyte (Li6.5 La2.5 Ba0.5 Nb Zr O12(LLBNZO)) and sintered the pallets of as-prepared material at elevated temperature like 1050, 1100, 1150 and 1200 °C. The objective to carry out this research was to observe the effect of temperature on porosity, density and transport properties of materials. Preliminary results suggest that the material sintered at higher temperature could show enhanced performance in terms of fast ionic transport. This enhancement in performance can be attributed to low porosity of materials which is result of high temperature sintering.

Keywords: solid state battery, electrolyte, garnet structures, Li-ion battery

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8411 Synthesis, Structure and Functional Characteristics of Solid Electrolytes Based on Lanthanum Niobates

Authors: Maria V. Morozova, Yulia V. Emelyanova, Anastasia A. Levina, Elena S. Buyanova, Zoya A. Mikhaylovskaya, Sofia A. Petrova


The solid solutions of lanthanum niobates substituted by yttrium, bismuth and tungsten were synthesized. The structure of the solid solutions is either LaNbO4-based monoclinic or BiNbO4-based triclinic. The series where niobium is substituted by tungsten on B site reveals phase-modulated structure. The values of cell parameters decrease with increasing the dopant concentration for all samples except the tungsten series although the latter show higher total conductivity.

Keywords: impedance spectroscopy, LaNbO4, lanthanum ortho-niobates, solid electrolyte

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8410 Medium Composition for the Laboratory Production of Enzyme Fructosyltransferase (FTase)

Authors: O. R. Raimi, A. Lateef


Inoculum developments of A. niger were used for inoculation of medium for submerged fermentation and solid state fermentation. The filtrate obtained were used as sources of the extra-cellular enzymes. The FTase activities and the course of pH in submerged fermentation ranged from 7.53-24.42µ/ml and 4.4-4.8 respectively. The maximum FTase activity was obtained at 48 hours fermentation. In solid state fermentation, FTase activities ranged from 2.41-27.77µ/ml. Using ripe plantain peel and kola nut pod respectively. Both substrates supported the growth of the fungus, producing profuse growth during fermentation. In the control experiment (using kolanut pod) that lack supplementation, appreciable FTase activity of 16.92µ/ml was obtained. The optimum temperature range was 600C. it was also active at broad pH range of 1-9 with optimum obtain at pH of 5.0. FTase was stable within the range of investigated pH showing more than 60% activities. FTase can be used in the production of fructooligosaccharide, a functional food.

Keywords: Aspergillus niger, solid state fermentation, kola nut pods, Fructosyltransferase (FTase)

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8409 Synthesis and Characterization of Ferromagnetic Ni-Cu Alloys for Thermal Rectification Applications

Authors: Josue Javier Martinez Flores, Jaime Alvarez Quintana


A thermal rectifier consists of a device which can load a different heat flow which depends on the direction of that flow. That device is a thermal diode. It is well known that heat transfer in solids basically depends on the electrical, magnetic and crystalline nature of materials via electrons, magnons and phonons as thermal energy carriers respectively. In the present research, we have synthesized polycrystalline Ni-Cu alloys and identified the Curie temperatures; and we have observed that by way of secondary phase transitions, it is possible manipulate the heat conduction in solid state thermal diodes via transition temperature. In this sense, we have succeeded in developing solid state thermal diodes with a control gate through the Curie temperature via the activation and deactivation of magnons in Ni-Cu ferromagnetic alloys at room temperature. Results show thermal diodes with thermal rectification factors up to 1.5. Besides, the performance of the electrical rectifiers can be controlled by way of alloy Cu content; hence, lower Cu content alloys present enhanced thermal rectifications factors than higher ones.

Keywords: thermal rectification, Curie temperature, ferromagnetic alloys, magnons

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8408 Fire Smoke Removal over Cu-Mn-Ce Oxide Catalyst with CO₂ Sorbent Addition: Co Oxidation and in-situ CO₂ Sorption

Authors: Jin Lin, Shouxiang Lu, Kim Meow Liew


In a fire accident, fire smoke often poses a serious threat to human safety especially in the enclosed space such as submarine and space-crafts environment. Efficient removal of the hazardous gas products particularly a large amount of CO and CO₂ gases from these confined space is critical for the security of the staff and necessary for the post-fire environment recovery. In this work, Cu-Mn-Ce composite oxide catalysts coupled with CO₂ sorbents were prepared using wet impregnation method, solid-state impregnation method and wet/solid-state impregnation method. The as-prepared samples were tested dynamically and isothermally for CO oxidation and CO₂ sorption and further characterized by the X-ray diffraction (XRD), nitrogen adsorption and desorption, and field emission scanning electron microscopy (FE-SEM). The results showed that all the samples were able to catalyze CO into CO₂ and capture CO₂ in situ by chemisorption. Among all the samples, the sample synthesized by the wet/solid-state impregnation method showed the highest catalytic activity toward CO oxidation and the fine ability of CO₂ sorption. The sample prepared by the solid-state impregnation method showed the second CO oxidation performance, while the coupled sample using the wet impregnation method exhibited much poor CO oxidation activity. The various CO oxidation and CO₂ sorption properties of the samples might arise from the different dispersed states of the CO₂ sorbent in the CO catalyst, owing to the different preparation methods. XRD results confirmed the high-dispersed sorbent phase in the samples prepared by the wet and solid impregnation method, while that of the sample prepared by wet/solid-state impregnation method showed the larger bulk phase as indicated by the high-intensity diffraction peaks. Nitrogen adsorption and desorption results further revealed that the latter sample had a higher surface area and pore volume, which were beneficial for the CO oxidation over the catalyst. Hence, the Cu-Mn-Ce oxide catalyst coupled with CO₂ sorbent using wet/solid-state impregnation method could be a good choice for fire smoke removal in the enclosed space.

Keywords: CO oxidation, CO₂ sorption, preparation methods, smoke removal

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8407 Production of Biodiesel Using Tannery Fleshing as a Feedstock via Solid-State Fermentation

Authors: C. Santhana Krishnan, A. M. Mimi Sakinah, Lakhveer Singh, Zularisam A. Wahid


This study was initiated to evaluate and optimize the conversion of animal fat from tannery wastes into methyl ester. In the pre-treatment stage, animal fats feedstock was hydrolysed and esterified through solid state fermentation (SSF) using Microbacterium species immobilized onto sand silica matrix. After 72 hours of fermentation, predominant esters in the animal fats were found to be with 83.9% conversion rate. Later, esterified animal fats were transesterified at 3 hour reaction time with 1% NaOH (w/v %), 6% methanol to oil ratio (w/v %) to produce 89% conversion rate. C13 NMR revealed long carbon chain in fatty acid methyl esters at 22.2817-31.9727 ppm. Methyl esters of palmitic, stearic, oleic represented the major components in biodiesel.

Keywords: tannery wastes, fatty animal fleshing, trans-esterification, immobilization, solid state fermentation

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8406 Municipal Solid Waste Management Characteristics and Management Challenges in Bauchi Metropolitan Area, Nigeria

Authors: Haruna Abdu Usman, Bashir Usman Mohammed, Mohammed Umar Jamil


Municipal solid waste management constitutes a serious problem bedeviling environmental protection agencies in many cities of developing countries. Most agencies do not collect the totality of the waste generated in their cities. This study presents the current solid waste management practices and problems in Bauchi metropolis, Bauchi state Nigeria. The general feature is characterized by inefficient, insufficient and irrational collection and improper disposal alternatives. The consequent environmental effects of these problems depict clogged city drains, uncollected heap of waste on road sides of residential areas, vacant plots and uncompleted buildings and highways. This contributes immensely to flooding in the city. The major challenges facing the state environmental protection agency includes; lack of collection and disposal points, technical and institutional arrangements, financial resources and general attitude of the serving public among others. The study suggested a comprehensive and integrated approach to the solid waste management which recognizes and incorporates the interventionist role of the state government, the private formal and informal waste management operators and the serving public.

Keywords: municipal solid waste, bauchi metropolitan area, environmental protection agency, solid waste management, waste disposal

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8405 Optimizing Cellulase Production from Municipal Solid Wastes (MSW) Following a Solid State Fermentation (SSF) by Trichoderma reesei and Aspergillus niger

Authors: Jwan J. Abdullah, Greetham Darren, Gregory A, Tucker, Chenyu Du


Solid-state fermentation (SSF) is an alternative to liquid fermentations for the production of commercially important products such as antibiotics, single cell proteins, enzymes, organic acids, or biofuels from lignocellulosic material. This paper describes the optimisation of SSF on municipal solid waste (MSW) for the production of cellulase enzyme. Production of cellulase enzymes was optimised by Trichoderma reesei or Aspergillus niger for temperature, moisture content, inoculation, and period of incubation. Also, presence of minerals, and alternative carbon and nitrogen sources. Optimisation revealed that production of cellulolytic enzymes was optimal when using Trichoderma spp at 30°C with an incubation period of 168 hours with a 60% moisture content. Crude enzymes produced from MSW, by Trichoderma were evaluated for the saccharification of MSW and compared with activity of a commercially available enzyme, results demonstrated that MSW can be used as inexpensive lignocellulosic material for the production of cellulase enzymes using Trichoderma reesei.

Keywords: SSF, enzyme hydrolysis, municipal solid waste (MSW), optimizing conditions, enzyme hydrolysis

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8404 Assessment of Solid Waste Management in General Mohammed Inuwa Wushishi Housing Estate, Minna, Niger State, Nigeria

Authors: Garba Inuwa Kuta, Mohammed, Adamu, Mohammed Ahmed Emigilati, Ibrahim Ishiaku, Kudu Dangana


The study sought to identify the problems of solid waste management in General Mohammed InuwaWushishi Housing Estate. The two broad types of data, the secondary and primary data were used in the study. Questionnaires and personal observations were also used to collect some of the data. Factors impeding the effective and efficient solid waste management were identified. The study revealed that sacks disposal method and open dumping are the most commonly used method of disposal, about 30.0% of the respondent use sacks disposal method in the estate while 24.9% dump their refuse on the floor. Wrong attitudes and perceptions of the people about sanitation issues contributed to solid waste management problems of General Mohammed InuwaWushishi Housing Estate. Majority of the households did not educate their members on the need to clean their surroundings and refuse to buy drum for waste disposal from Niger State Environmental Protection Agency (NISEPA) on the basis that the drums are expensive. Virtually, all the people depended on Niger State Environmental Protection Agency (NISEPA) facilities for the disposal of their household refuse. Solid waste management problems were partly the results of NISEPA’s inability to cope with the situation because of lack of equipment. It was recommended that there should be an increase in enlightenment to the people on domestic waste disposal to keep the surroundings clean.

Keywords: housing estate, assessment, solid waste, disposal, management

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8403 Reuse of Municipal Solid Waste Incinerator Fly Ash for the Synthesis of Zeolite: Effects of Different Operation Conditions

Authors: Jyh-Cherng Chen, Yi-Jie Lin


This study tries to reuse the fly ash of municipal solid waste incinerator (MSWI) for the synthesis of zeolites. The fly ashes were treated with NaOH alkali fusion at different temperatures for 40 mins and then synthesized the zeolites with hydrothermal method at 105oC for different operation times. The effects of different operation conditions and the optimum synthesis parameters were explored. The specific surface area, surface morphology, species identification, adsorption capacity, and the reuse potentials of the synthesized zeolites were analyzed and evaluated. Experimental results showed that the optimum operation conditions for the synthesis of zeolite from the mixed fly ash were Si/Al=20, alkali/ash=1.5, alkali fusion reaction with NaOH at 800oC for 40 mins, hydrolysis with L/S=200 at 105oC for 24 hr, and hydrothermal synthesis at 105oC for 48 hr. The largest specific surface area of synthesized zeolite could be increased to 943.05m2/g. The influence of different operation parameters on the synthesis of zeolite from mixed fly ash followed the sequence of Si/Al > hydrolysis L/S> hydrothermal time > alkali fusion temperature > alkali/ash ratio. The XRD patterns of synthesized zeolites were identified to be similar with the ZSM-23 zeolite. The adsorption capacities of synthesized zeolite for pollutants were increased as rising the specific surface area of synthesized zeolite. In summary, MSWI fly ash can be treated and reused to synthesize the zeolite with high specific surface area by the alkali fusion and hydrothermal method. The zeolite can be reuse for the adsorption of various pollutants. They have great potential for development.

Keywords: alkali fusion, hydrothermal, fly ash, zeolite

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8402 Iron Doped Biomaterial Calcium Borate: Synthesis and Characterization

Authors: G. Çelik Gül, F. Kurtuluş


Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA). 

Keywords: colemanite, conventional synthesis, powder x-ray diffraction, borates

Procedia PDF Downloads 249