Search results for: (FTIR) spectroscopy

Authors: Oiane Ruiz de Azua, Salvador Borros, Nuria Agullo, Jordi Arbusa

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Tackiness is described as the ability to spontaneously form a bond to another material under light pressures within a short application time. During the first few minutes of the adhesive's curing, it is necessary to have enough tack to keep the substrates together while cohesion is increasing within the adhesive. This property plays a key role in the manufacturing process of pieces. Epoxy adhesives, unlike other adhesives, usually present low tackiness before curing; however, there is very little literature about the use of tackifiers in epoxy adhesives, except for the high molecular weight epoxy additives. In the present work, a tetrafunctional epoxy resin based on Bisphenol-A and Sulfanilamide has been synthesized in order to be used as a tackifier. This additive offers improved specific adhesion to two-component (2K) epoxy adhesives. The dosage of the tackifier has to be done carefully not to alter the mechanical and rheological properties of the adhesive. The synthetized product has been analyzed by FTIR and ¹H-NMR analysis, and the effect of the addition of 1 wt % of the tackifier on rheological properties, viscoelastic behavior, and mechanical properties has been studied. On one hand, the addition of the product in the epoxy resin part showed a significant increase in tackiness regarding the neat epoxy resin. On the other hand, tackiness of the whole formulation was also increased. Curing time of the adhesive has not undergone any relevant changes with the tackifier addition. Regarding viscoelastic properties, Storage Modulus (G') and Loss Modulus (G'') remain also unchanged at ambient temperature. Probably, in case higher tackifier concentration would be added, differences in viscoelastic properties would be observed. The study of mechanical properties shows that hardness and tensile strength also keep their values unchanged regarding neat two component adhesive. In conclusion, the addition of 1 wt % of sulfanilamide/epoxy enhanced the tackiness of the epoxy resin part, improves tack without modifying significantly either the rheological, the mechanical, or the viscoelastic properties of the product. Thus, the sulfanilamide presented could be a good candidate to be used as an additive to the 2k epoxy formulation for the manufacturing process of pieces.

Keywords: epoxy adhesive, manufacturing process of pieces, sulfanilamide, tackifiers

Procedia PDF Downloads 174

Authors: Serkan Sayin, Songul F. Varol

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High attention on the organic light-emitting diodes has been paid since their efficient properties in the flat panel displays, and solid-state lighting was realized. Because of their high efficient electroluminescence, brightness and providing eminent in the emission range, organic light emitting diodes have been preferred a material compared with the other materials consisting of the liquid crystal. Calixarenes obtained from the reaction of p-tert-butyl phenol and formaldehyde in a suitable base have been potentially used in various research area such as catalysis, enzyme immobilization, and applications, ion carrier, sensors, nanoscience, etc. In addition, their tremendous frameworks, as well as their easily functionalization, make them an effective candidate in the applied chemistry. Herein, a calix[4]arene derivative has been synthesized, and its structure has been fully characterized using Fourier Transform Infrared Spectrophotometer (FTIR), proton nuclear magnetic resonance (¹H-NMR), carbon-13 nuclear magnetic resonance (¹³C-NMR), liquid chromatography-mass spectrometry (LC-MS), and elemental analysis techniques. The calixarene derivative has been employed as an emitting layer in the fabrication of the organic light-emitting diodes. The optical and electrochemical features of calixarane-contained organic light-emitting diodes (Clx-OLED) have been also performed. The results showed that Clx-OLED exhibited blue emission and high external quantum efficacy. As a conclusion obtained results attributed that the synthesized calixarane derivative is a promising chromophore with efficient fluorescent quantum yield that provides it an attractive candidate for fabricating effective materials for fluorescent probes and labeling studies. This study was financially supported by the Scientific and Technological Research Council of Turkey (TUBITAK Grant no. 117Z402).

Keywords: calixarene, OLED, supramolecular chemistry, synthesis

Procedia PDF Downloads 249

Authors: Tichaona Nharingo, Hope Tauya, Mambo Moyo

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Wood ash has been demonstrated to have favourable adsorption capacity for heavy metal ions but suffers the application problem of difficult to separate/isolate from the batch adsorption systems. Fabrication of wood ash beads using multifunctional group and non-toxic carbohydrate, alginate, may improve the applicability of wood ash in environmental pollutant remediation. In this work, alginate-wood ash beads (AWAB) were fabricated and applied to the removal of cadmium ions from aqueous systems. The beads were characterized by FTIR, TGA/DSC, SEM-EDX and their pHZPC before and after the adsorption of Cd(II) ions. Important adsorption parameters i.e. pH, AWAB dosage, contact time and ionic strength were optimized and the effect of initial concentration of Cd(II) ions to the adsorption process was established. Adsorption kinetics, adsorption isotherms, adsorption mechanism and application of AWAB to real water samples spiked with Cd(II) ions were ascertained. The composite adsorbent was characterized by a heterogeneous macro pore surface comprising of metal oxides, multiple hydroxyl groups and carbonyl groups that were involved in electrostatic interaction and Lewis acid-base interactions with the Cd(II) ions. The pseudo second order and the Freundlich isotherm models best fitted the adsorption kinetics and isotherm data respectively suggesting chemical sorption process and surface heterogeneity. The presence of Pb(II) ions inhibited the adsorption of Cd(II) ions (reduced by 40 %) attributed to the competition for the adsorption sites. The Cd(II) loaded beads could be regenerated using 0.1 M HCl and could be applied to four sorption-desorption cycles without significant loss in its initial adsorption capacity. The high maximum adsorption capacity, stability, selectivity and reusability of AWAB make the adsorbent ideal for application in the removal of Cd(II) ions from real water samples. Column type adsorption experiments need to be explored to establish the potential of the adsorbent in removing Cd(II) ions using continuous flow systems.

Keywords: adsorption, Cd(II) ions, regeneration, wastewater, wood ash-alginate beads

Procedia PDF Downloads 238

Authors: Ayesha Asma, Aqsa Arooj

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It is an essential need in this era of Science and Technology to investigate some unique and appropriate materials for optoelectronic applications. Here, we deliberated, for the first time, the structural, optoelectronic, mechanical, vibrational, and thermo dynamical properties of hexagonal structure selenium-based ternary chalcogenides AScSe₂ (A= K, Cs) by using Perdew-Burke-Ernzerhof Generalized-Gradient-Approximation (PBE-GGA). The lattice angles for these materials are found as α=β=90o and γ=120o. KScSe₂ optimized with lattice parameters a=b=4.3 (Å), c=7.81 (Å) whereas CsScSe₂ got relaxed at a=b=4.43 (Å) and c=8.51 (Å). However, HSE06 functional has overestimated the lattice parameters to the extent that for KScSe₂ a=b=4.92 (Å), c=7.10 (Å), and CsScSe₂ a=b=5.15 (Å), c=7.09 (Å). The energy band gap of these materials calculated via PBE-GGA and HSE06 functionals confirms their semiconducting nature. Concerning Born’s criteria, these materials are mechanically stable ones. Moreover, the temperature dependence of thermodynamic potentials and specific heat at constant volume are also determined while using the harmonic approximation. The negative values of free energy ensure their thermodynamic stability. The vibrational modes are calculated by plotting the phonon dispersion and the vibrational density of states (VDOS), where infrared (IR) and Raman spectroscopy are used to characterize the vibrational modes. The various optical parameters are examined at a smearing value of 0.5eV. These parameters unveil that these materials are good absorbers of incident light in ultra-violet (UV) regions and may be utilized in photovoltaic applications.

Keywords: structural, optimized, vibrational, ultraviolet

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Authors: Shyam Ranjan Kumar, Shashikant Rajpal

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Zinc Telluride (ZnTe) is a binary II-VI direct band gap semiconducting material. This semiconducting material has several applications in sensors, photo-electrochemical devices and photovoltaic solar cell. In this study, Zinc telluride (ZnTe) thin films were deposited on nickel substrate by electrodeposition technique using potentiostat/galvanostat at -0.85 V using AR grade of Zinc Chloride (ZnCl2), Tellurium Tetrachloride (TeCl4) in non-aqueous bath. The developed films were physically stable and showed good adhesion. The as deposited ZnTe films were annealed at 400ºC in air. The solid state properties and optical properties of the as deposited and annealed films were carried out by XRD, EDS, SEM, AFM, UV–Visible spectrophotometer, and photoluminescence spectrophotometer. The diffraction peak observed at 2θ = 49.58° with (111) plane indicate the crystalline nature of ZnTe film. Annealing improves the crystalline nature of the film. Compositional analysis reveals the presence of Zn and Te with tellurium rich ZnTe film. SEM photograph at 10000X shows that grains of film are spherical in nature and densely distributed over the surface. The average roughness of the film is measured by atomic force microscopy and it is nearly equal to 60 nm. The direct wide band gap of 2.12 eV is observed by UV-Vis spectroscopy. Luminescence peak of the ZnTe films are also observed in as deposited and annealed case.

Keywords: annealing, electrodeposition, optical properties, thin film, XRD, ZnTe

Procedia PDF Downloads 187

Authors: Joanna Skopinska-Wisniewska, Anna Bajek, Marta Ziegler-Borowska, Alina Sionkowska

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Hydrogels are a class of materials widely used in medicine for many years. Proteins, such as collagen, due to the presence of a large number of functional groups are easily wettable by polar solvents and can create hydrogels. The supramolecular network capable to swelling is created by cross-linking of the biopolymers using various reagents. Many cross-linking agents has been tested for last years, however, researchers still are looking for a new, more secure reactants. Squaric acid, 3,4-dihydroxy 3-cyclobutene 1,2- dione, is a very strong acid, which possess flat and rigid structure. Due to the presence of two carboxyl groups the squaric acid willingly reacts with amino groups of collagen. The main purpose of this study was to investigate the influence of addition of squaric acid on the chemical, physical and biological properties of collagen materials. The collagen type I was extracted from rat tail tendons and 1% solution in 0.1M acetic acid was prepared. The samples were cross-linked by the addition of 5%, 10% and 20% of squaric acid. The mixtures of all reagents were incubated 30 min on magnetic stirrer and then dialyzed against deionized water. The FTIR spectra show that the collagen structure is not changed by cross-linking by squaric acid. Although the mechanical properties of the collagen material deteriorate, the temperature of thermal denaturation of collagen increases after cross-linking, what indicates that the protein network was created. The lyophilized collagen gels exhibit porous structure and the pore size decreases with the higher addition of squaric acid. Also the swelling ability is lower after the cross-linking. The in vitro study demonstrates that the materials are attractive for 3T3 cells. The addition of squaric acid causes formation of cross-ling bonds in the collagen materials and the transparent, stiff hydrogels are obtained. The changes of physicochemical properties of the material are typical for cross-linking process, except mechanical properties – it requires further experiments. However, the results let us to conclude that squaric acid is a suitable cross-linker for protein materials for medicine and tissue engineering.

Keywords: collagen, squaric acid, cross-linking, hydrogel

Procedia PDF Downloads 384

Authors: M. S. Ashraf, Raja Rizwan Hussain, A. M. Alhozaimy, A. I. Al-Negheimish

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The effect of supplementary cementitious materials (SCMs) with concrete pore solution on the protective properties of the oxide films that form on reinforcing steel bars has been experimentally investigated using electrochemical impedance spectroscopy (EIS) and Tafel Scan. The tests were conducted on oxide films grown in saturated calcium hydroxide solutions that included different representative amounts of NaOH and KOH which are the compounds commonly observed in ordinary portland cement concrete pore solution. In addition to that, commonly used mineral admixtures (silica fume, natural pozzolan and fly ash) were also added to the simulated concrete pore solution. The results of electrochemical tests show that supplementary cementitious materials do have an effect on the protective properties of the passive oxide film. In particular, silica fume has been shown to have a negative influence on the film quality though it has positive effect on the concrete properties. Fly ash and natural pozzolan increase the protective qualities of the passive film. The research data in this area is very limited in the past and needed further investigation.

Keywords: supplementary cementitious materials (SCMs), passive film, EIS, Tafel scan, rebar, concrete, simulated concrete pore solution (SPS)

Procedia PDF Downloads 390

Authors: Alparslan A. Balta, Hilmi Yurdakul, Orkun Tunckan, Servet Turan, Arife Yurdakul

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A silicon oxynitride (Si2N2O), the mineralogical name is “Sinoite”, reveals the outstanding physical, mechanical and thermal properties, e.g., good oxidation resistance at high temperatures, high fracture toughness with rod shape, high hardness, low theoretical density, good thermal shock resistance by low thermal expansion coefficient and high thermal conductivity. In addition, the orthorhombic crystal structure of Si2N2O allows accommodating the rare earth (RE) element atoms along the “c” axis due to existing large structural interstitial sites. Here, 0.02 to 0.12 wt. % Nd3+ doped Si2N2O samples were successfully synthesized by spark plasma sintering (SPS) method at 30MPa pressure and 1650oC temperature. Li2O was also utilized as a sintering additive to take advantage of low eutectic point during synthesizing. The specimens were characterized in detail by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and cathodoluminescence (CL) in SEM and photoluminescence (PL) spectroscopy. Based on the overall results, the Si2N2O phase was obtained above 90% by the SPS route. Furthermore, Nd3+: Si2N2O samples showed a very broad intense emission peak between 400-700 nm, which corresponds to white color. Therefore, this material can be considered as a promising candidate for white light-emitting diodes (WLEDs) purposes. This study was supported by TUBITAK under project number 217M667.

Keywords: neodymium, oxynitride, Si₂N₂O, WLEDs

Procedia PDF Downloads 131

Authors: Reza Eslami-Farsani, Hamed Khosravi, Saba Fayazzadeh

Abstract:

Lightweight and efficient structures have the aim to enhance the efficiency of the components in various industries. Toward this end, composites are one of the most widely used materials because of durability, high strength and modulus, and low weight. One type of the advanced composites is grid-stiffened composite (GSC) structures which have been extensively considered in aerospace, automotive, and aircraft industries. They are one of the top candidates for replacing some of the traditional components which are used here. Although there are a good number of published surveys on the design aspects and fabrication of GSC structures, little systematic work has been reported on their material modification to improve their properties, to our knowledge. Matrix modification using nanoparticles is an effective method to enhance the flexural properties of the fibrous composites. In the present study, a silane coupling agent (3-glycidoxypropyltrimethoxysilane/3-GPTS) was introduced onto the silica (SiO2) nanoparticle surface and its effects on the three-point flexural response of isogrid E-glass/epoxy composites were assessed. Based on the fourier transform infrared spectrometer (FTIR) spectra, it was inferred that the 3-GPTS coupling agent was successfully grafted onto the surface of SiO2 nanoparticles after modification. Flexural test revealed an improvement of 16%, 14%, and 36% in stiffness, maximum load and energy absorption of the isogrid specimen filled with 3 wt.% 3-GPTS/SiO2 compared to the neat one. It would be worth mentioning that in these structures, a considerable energy absorption was observed after the primary failure related to the load peak. Also, 3-GPTMS functionalization had a positive effect on the flexural behavior of the multiscale isogrid composites. In conclusion, this study suggests that the addition of modified silica nanoparticles is a promising method to improve the flexural properties of the grid-stiffened fibrous composite structures.

Keywords: isogrid-stiffened composite panels, silica nanoparticles, surface modification, flexural properties, energy absorption

Procedia PDF Downloads 243

Authors: Motwkel M. Alhaj, Bashir M. Elhassan

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

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

Procedia PDF Downloads 107

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

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

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

Procedia PDF Downloads 192

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

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

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

Procedia PDF Downloads 311

Authors: Reza Eslami-Farsani, Hamed Khosravi, Saba Fayazzadeh

Abstract:

Lightweight and efficient structures have the aim to enhance the efficiency of the components in various industries. Toward this end, composites are one of the most widely used materials because of durability, high strength and modulus, and low weight. One type of the advanced composites is grid-stiffened composite (GSC) structures, which have been extensively considered in aerospace, automotive, and aircraft industries. They are one of the top candidates for replacing some of the traditional components, which are used here. Although there are a good number of published surveys on the design aspects and fabrication of GSC structures, little systematic work has been reported on their material modification to improve their properties, to our knowledge. Matrix modification using nanoparticles is an effective method to enhance the flexural properties of the fibrous composites. In the present study, a silane-coupling agent (3-glycidoxypropyltrimethoxysilane/3-GPTS) was introduced onto the silica (SiO2) nanoparticle surface and its effects on the three-point flexural response of isogrid E-glass/epoxy composites were assessed. Based on the fourier transform infrared spectrometer (FTIR) spectra, it was inferred that the 3-GPTS coupling agent was successfully grafted onto the surface of SiO2 nanoparticles after modification. Flexural test revealed an improvement of 16%, 14%, and 36% in stiffness, maximum load and energy absorption of the isogrid specimen filled with 3 wt.% 3-GPTS/SiO2 compared to the neat one. It would be worth mentioning that in these structures, considerable energy absorption was observed after the primary failure related to the load peak. In addition, 3-GPTMS functionalization had a positive effect on the flexural behavior of the multiscale isogrid composites. In conclusion, this study suggests that the addition of modified silica nanoparticles is a promising method to improve the flexural properties of the grid-stiffened fibrous composite structures.

Keywords: isogrid-stiffened composite panels, silica nanoparticles, surface modification, flexural properties

Procedia PDF Downloads 232

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

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

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

Procedia PDF Downloads 67

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

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

Keywords: biosensor, glycan, lectin, prostate cancer

Procedia PDF Downloads 367

Authors: Lucky Malise, Hilary Rutto, Tumisang Seodigeng

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Heavy metal contamination in waste water is a very serious issue affecting a lot of industrialized countries due to the health and environmental impact of these heavy metals on human life and the ecosystem. Adsorption using activated carbon is the most promising method for the removal of heavy metals from waste water but commercial activated carbon is expensive which gives rise to the need for alternatively activated carbon derived from cheap precursors, agricultural wastes, or byproducts from other processes. In this study activated bio-carbon derived from the carbonaceous material obtained from the pyrolysis of Marula nut shells was chemically activated and used as an adsorbent for the removal of lead (II) and copper (II) ions from aqueous solution. The surface morphology and chemistry of the adsorbent before and after chemical activation with zinc chloride impregnation were studied using SEM and FTIR analysis respectively and the results obtained indicate that chemical activation with zinc chloride improves the surface morphology of the adsorbent and enhances the intensity of the surface oxygen complexes on the surface of the adsorbent. The effect of process parameters such as adsorbent dosage, pH value of the solution, initial metal concentration, contact time, and temperature on the adsorption of lead (II) and copper (II) ions onto Marula nut activated carbon were investigated, and their optimum operating conditions were also determined. The experimental data was fitted to both the Langmuir and Freundlich isotherm models, and the data fitted best on the Freundlich isotherm model for both metal ions. The adsorption kinetics were also evaluated, and the experimental data fitted the pseudo-first order kinetic model better than the pseudo second-order kinetic model. The adsorption thermodynamics were also studied and the results indicate that the adsorption of lead and copper ions is spontaneous and exothermic in nature, feasible, and also involves a dissociative mechanism in the temperature range of 25-45 °C.

Keywords: adsorption, isotherms, kinetics, marula nut shells activated carbon, thermodynamics

Procedia PDF Downloads 262

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

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

Keywords: dissolution, disaggregation, Lamotrigine, bioequivalence

Procedia PDF Downloads 449

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

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

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

Procedia PDF Downloads 350

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

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

Keywords: antipathogenic activity, ascorbic acid, cytotoxicity, stability

Procedia PDF Downloads 140

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

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

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

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

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

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

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

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

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

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

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

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

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Authors: Ranjot Kaur, Om P. Katare, Anupama Sharma, Sarah R. Dennison, Kamalinder K. Singh, Bhupinder Singh

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Respiratory microbial infections being among the top leading cause of death worldwide are difficult to treat as the microbes reside deep inside the airways, where only a small fraction of drug can access after traditional oral or parenteral routes. As a result, high doses of drugs are required to maintain drug levels above minimum inhibitory concentrations (MIC) at the infection site, unfortunately leading to severe systemic side-effects. Therefore, delivering antimicrobials directly to the respiratory tract provides an attractive way out in such situations. In this context, current study embarks on the systematic development of lung lia pid-modified chitosan nanoparticles for inhalation of voriconazole. Following the principles of quality by design, the chitosan nanoparticles were prepared by ionic gelation method and further coated with major lung lipid by precipitation method. The factor screening studies were performed by fractional factorial design, followed by optimization of the nanoparticles by Box-Behnken Design. The optimized formulation has a particle size range of 170-180nm, PDI 0.3-0.4, zeta potential 14-17, entrapment efficiency 45-50% and drug loading of 3-5%. The presence of a lipid coating was confirmed by FESEM, FTIR, and X-RD. Furthermore, the nanoparticles were found to be safe upto 40µg/ml on A549 and Calu-3 cell lines. The quantitative and qualitative uptake studies also revealed the uptake of nanoparticles in lung epithelial cells. Moreover, the data from Spraytec and next-generation impactor studies confirmed the deposition of nanoparticles in lower airways. Also, the interaction of nanoparticles with DPPC monolayers signifies its biocompatibility with lungs. Overall, the study describes the methodology and potential of lipid-coated chitosan nanoparticles in futuristic inhalation nanomedicine for the management of pulmonary aspergillosis.

Keywords: dipalmitoylphosphatidylcholine, nebulization, DPPC monolayers, quality-by-design

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Authors: M. Jerold, V. Sivasubramanian

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

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

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

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

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

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Authors: Mangaka C. Matoetoe, Fredrick O. Okumu

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

Keywords: kinetics, morphology, nanoparticles, platinum, silver

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Authors: Kefyalew Muleta, Tetemke Mehari

Abstract:

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

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

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

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

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

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Authors: E. A. Alshaafi, A. Prakash

Abstract:

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

Keywords: ultrasonic techniques, emulsion, characterization, droplet size

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