Search results for: calorimetry

Authors: Rhoda Afriyie Mensah, Lin Jiang, Solomon Asante-Okyere, Xu Qiang, Cong Jin

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Flammability analysis of extruded polystyrene (XPS) has become crucial due to its utilization as insulation material for energy efficient buildings. Using the Kissinger-Akahira-Sunose and Flynn-Wall-Ozawa methods, the degradation kinetics of two pure XPS from the local market, red and grey ones, were obtained from the results of thermogravity analysis (TG) and microscale combustion calorimetry (MCC) experiments performed under the same heating rates. From the experiments, it was discovered that red XPS released more heat than grey XPS and both materials showed two mass loss stages. Consequently, the kinetic parameters for red XPS were higher than grey XPS. A comparative evaluation of activation energies from MCC and TG showed an insignificant degree of deviation signifying an equivalent apparent activation energy from both methods. However, different activation energy profiles as a result of the different chemical pathways were presented when the dependencies of the activation energies on extent of conversion for TG and MCC were compared.

Keywords: flammability, microscale combustion calorimetry, thermogravity analysis, thermal degradation, kinetic analysis

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Authors: Maryam Nejat Dehkordi, Per Lincoln, Hassan Momtaz

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Interaction of Schiff base complexes of iron and manganese (iron [N, N’ Bis (5-(triphenyl phosphonium methyl) salicylidene) -1, 2 ethanediamine) chloride, [Fe Salen]Cl, manganese [N, N’ Bis (5-(triphenyl phosphonium methyl) salicylidene) -1, 2 ethanediamine) acetate) with DNA were investigated by spectroscopic and isothermal titration calorimetry techniques (ITC). The absorbance spectra of complexes have shown hyper and hypochromism in the presence of DNA that is indication of interaction of complexes with DNA. The linear dichroism (LD) measurements confirmed the bending of DNA in the presence of complexes. Furthermore, isothermal titration calorimetry experiments approved that complexes bound to DNA on the base of both electrostatic and hydrophobic interactions. Furthermore, ITC profile exhibits the existence of two binding phases for the complex. Antibacterial activity of ligand and complexes were tested in vitro to evaluate their activity against the gram positive and negative bacteria.

Keywords: Schiff base complexes, ct-DNA, linear dichroism (LD), isothermal titration calorimetry (ITC), antibacterial activity

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Authors: Sumara Khursheed, Jitendra Sharma

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The present work reports synthesis of nanocomposites (NCs) of phosphor (KCaVO4:Sm3+) embedded poly(methylmethacrylate) (PMMA) using solution casting method and their optical properties measurements for their possible application in making flexible luminescent films. X-ray diffraction analyses were employed to obtain the structural parameters as crystallinity, shape and size of the obtained NCs. The emission and excitation spectra were obtained using Photoluminescence spectroscopy to quantify the spectral properties of these fluorescent polymer/phosphor films. Optical energy gap has been estimated using UV-VIS spectroscopy while differential scanning calorimetry (DSC) was exploited to measure the thermal properties of the NC films in terms of their thermal stability, glass transition temperature and degree of crystallinity etc.

Keywords: nanocomposites, luminescence, XRD, differential scanning calorimetry, PMMA

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Authors: Hang Tran, Victor Brial, Luca Sorelli, Claudiane Ouellet-Plamondon, David Conciatori, Laurent Birry

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Spend pot lining (SPL) is a by-product generated from primary aluminum production. SPL consists of two parts, the first cut is rich in carbonaceous materials, and the second cut is rich in aluminum and silicon oxides. After treating by the hydrometallurgical Low Caustic Leaching and Liming process, the refractory part of SPL becomes an inert material, called LCLL ash in this project. LCLL ash was calcined at different temperatures (800 and 1000°C) and Calcined LCLL ash ground as fines of cement and replacement a part of cement in concrete production. The effect of LCLL ash on the chemical properties, mechanical properties and fresh behavior of concrete was evaluated by isothermal calorimetry, compressive test, and slump test. These results were compared to the reference mixture.

Keywords: spend pot lining, concrete, cement, compressive strength, calorimetry

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Authors: Naveed Ahmad, Farooq Ahmad, Abdul Aal Al-Khazaal

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Rheology can be used as a tool to examine the crystallization kinetics of polymers and polymer composites, and it provides more accurate results than the commonly used conventional techniques like differential scanning calorimetry (DSC) when the crystallization kinetics are slow. Crystallization occurs when crystalline polymers are cooled below their thermodynamic melting point temperature. At the start of this process, there is a gradual change in the mechanical response of the material from the liquid to the solid state, which is due to the change at the microstructure level of the polymer and polymer composites. This is one of the main characteristics of the rheological methodology that sets it apart from the conventional DSC method. In the present work, we used both rheological and differential scanning calorimetric techniques to perform both isothermal and non-isothermal crystallization experiments on a range of syndiotactic polypropylenes/clay composites with varying doses of clay contents in order to investigate the crystallization behavior of the materials. The objective of this work is to explore the effect of clay contents on the crystallization behavior of the syndiotactic polypropylene/clay composites and to couple the rheological methods with more conventional techniques such as Differential Scanning Calorimetry (DSC). Time sweep tests at a constant heating rate of 40°C/minutes were used to investigate the crystallization kinetics using the Atomic Rheumetric Expansion System (ARES). Crystallization behavior was found to be strongly dependent on the clay contents of syndiotactic polypropylene/clay composites. Both melting point (Tₘ) and crystallization temperatures (T𝒸) were found to increase with an increase in clay contents. Excellent agreement is found between the results obtained by both the rheological and differential scanning calorimetric (DSC) methods.

Keywords: quiescent crystallization, polymer composites, rheology, differential scanning calorimetry, syndiotactic polypropylene/clay composites

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Authors: Adriana Souza M. Batista, Cláubia Pereira, Luiz O. Faria

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The irradiation of polymeric materials has received much attention because it can produce diverse changes in chemical structure and physical properties. Thus, studying the chemical and structural changes of polymers is important in practice to achieve optimal conditions for the modification of polymers. The effect of gamma irradiation on the crystalline structure of poly(vinylidene fluoride) (PVDF) has been investigated using differential scanning calorimetry (DSC) and X-ray diffraction techniques (XRD). Gamma irradiation was carried out in atmosphere air with doses between 100 kGy at 3,000 kGy with a Co-60 source. In the melting thermogram of the samples irradiated can be seen a bimodal melting endotherm is detected with two melting temperature. The lower melting temperature is attributed to melting of crystals originally present and the higher melting peak due to melting of crystals reorganized upon heat treatment. These results are consistent with those obtained by XRD technique showing increasing crystallinity with increasing irradiation dose, although the melting latent heat is decreasing.

Keywords: differential scanning calorimetry, gamma irradiation, PVDF, X-ray diffraction technique

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Authors: Pauline Ribert, Gaelle Roudaut, Sebastien Dupont, Laurent Beney

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Yeasts, anhydrobiotic organisms, can survive extreme water disturbances, thanks to the prolonged and reversible suspension of their cellular activity as well as the establishment of a defense arsenal. This property is exploited by many industrialists. One of the protection systems implemented by yeast is the vitrification of its cytoplasm by trehalose. The thermal resistance of dry yeasts is a crucial parameter for their use. However, studies on the thermal resistance of dry yeasts are often based on yeasts produced in laboratory conditions with non-optimal drying processes. We, therefore, propose a study on the thermal resistance of industrial dry yeasts in relation to their thermophysical properties. Heat stress was applied at three temperatures (50, 75, and 100°C) for 10, 30, or 60-minute treatments. The survival of yeasts to these treatments was estimated, and their thermophysical properties were studied by differential scanning calorimetry. The industrial dry yeasts resisted 60 minutes at 50°C and 75°C and 10 minutes at a temperature close to 100°C. At 100°C, yeast was above their glass transition temperature. Industrial dry yeasts are therefore capable of withstanding high thermal stress if maintained in a specific thermophysical state.

Keywords: dry yeast, glass transition, thermal resistance, vitrification

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Authors: Seyfullah Madakbas, Hatice Birtane, Memet Vezir Kahraman

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In this study, we aimed to synthesize and characterize polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite. Polyimide nanocomposites widely have been used in membranes in fuel cell, solar cell, gas filtration, sensors, aerospace components, printed circuit boards. Firstly, polyamic acid was synthesized and characterized by Fourier Transform Infrared. Then, polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite was prepared with thermal imidization method. The obtained polyimide nanocomposite was characterized by Fourier Transform Infrared, Scanning Electron Microscope, Thermal Gravimetric Analysis and Differential Scanning Calorimetry. Thermal stability of polyimide nanocomposite was evaluated by thermal gravimetric analysis and differential scanning calorimetry. Surface morphology of composite samples was investigated by scanning electron microscope. The obtained results prove that successfully prepared polyhedral oligomeric silsesquioxanes are containing polyimide nanocomposite. The obtained nanocomposite can be used in many industries such as electronics, automotive, aerospace, etc.

Keywords: polyimide, nanocomposite, polyhedral oligomeric silsesquioxanes

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Authors: Anton Trník, Lenka Scheinherrová, Robert Černý

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Silica fume is a by-product of the ferro-silicon and silicon metal industries. It is mainly in the form of amorphous silica. Silica fume belongs to pozzolanic active materials which can be used in concrete to improve its final properties. In this paper, the influence of silica fume on hydration of cement pastes is studied using differential scanning calorimetry (DSC) and thermogravimetry (TG) at various curing times (2, 7, 28, and 90 days) in the temperature range from 25 to 1000 °C in an argon atmosphere. Samples are prepared from Portland cement CEM I 42.5 R which is partially replaced with the silica fume of 4, 8, and 12 wt.%. The water/binder ratio is chosen as 0.5. It is identified and described the liberation of physically bound water, calcium–silicate–hydrates dehydration, portlandite and calcite decomposition in studied samples. Also, it is found out that an exothermic peak at 950 °C is observed without a significant mass change for samples with 12 wt.% of silica fume after two days of hydration. This peak is probably caused by the pozzolanic reaction between silica fume and Portland cement. Its size corresponds to the degree of crystallization between Ca and Si. The portlandite content is lower for the samples with a higher amount of silica fume.

Keywords: differential scanning calorimetry, hydration, silica fume, thermogravimetry

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Authors: Sharmila Pradhan, Ralf Lach, George Michler, Jean Mark Saiter, Rameshwar Adhikari

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Ethylene/1-octene copolymer was modified incorporating three types of nanofillers differed in their dimensionality in order to investigate the effect of filler dimensionality on mechanical properties, for instance, tensile strength, microhardness etc. The samples were prepared by melt mixing followed by compression moldings. The microstructure of the novel material was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) method and Transmission electron microscopy (TEM). Other important properties such as melting, crystallizing and thermal stability were also investigated via differential scanning calorimetry (DSC) and Thermogravimetry analysis (TGA). The FTIR and XRD results showed that the composites were formed by physical mixing. The TEM result supported the homogeneous dispersion of nanofillers in the matrix. The mechanical characterization performed by tensile testing showed that the composites with 1D nanofiller effectively reinforced the polymer. TGA results revealed that the thermal stability of pure EOC is marginally improved by the addition of nanofillers. Likewise, melting and crystallizing properties of the composites are not much different from that of pure.

Keywords: copolymer, differential scanning calorimetry, nanofiller, tensile strength

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Authors: Mahfoud Benzerzour, Mouhamadou Amar, Nor-edine Abriak

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In this study, a sediment was used as a secondary raw material in cement substitution with prior treatment. The treatment adopted is a physical treatment involving grinding and separation to obtain different fractions, using a dry method (1 mm, 250µm, 120µm) and washing method (250µm and 120µm). They were subsequently heat treated at temperatures of 650°C, 750°C and 850°C for 1 hour and 3 hours, in order to enable chemical activation by decarbonation or by pozzolanic activation of the material. Different characterization techniques were performed. The determination of main physical and chemical characteristics was obtained through multiple tests: particle size distribution, specific density, the BET surface area, the initial setting time and hydration heat calorimetry Langavant. The chemical tests include: ATG analysis, X-ray diffractometry (XRD) and X-ray fluorescence (XRF) which were used to quantify the fractions, phases and chemical elements present. Compression tests were performed conforming NF EN 196-1 French standard, over terms of 7 days - 14 days - 28 days and 60 days on all formulated mortars: reference mortar based on 100% CEM I 52.5N binder and cement substituted mortars with 8% and 15% by treated sediment. This clearly evidenced contribution due to the chemical activity which was confirmed by calorimetry monitoring and strength investigation.

Keywords: sediment, characterization, grinding, heat treatment, substitution

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Authors: A. M. T. Jacinto, M.O. Osi

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Tamarind has various medicinal properties among which is its antibacterial property. Its bark contains saponins, alkaloids, sesquiterpenes and tannins. It is rich in phlobapenes which is responsible for antibacterial property. The objective of the study was to determine which bark will produce the highest antibacterial property, develop it into a topical cream and evaluate its quality and characteristics. Powdered barks of Tamarind were extracted by soxhlet method using 70% acetone. Stem bark produced a higher yield than trunk bark (5.85 g vs. 4.73 g). It was found that the trunk bark was more sensitive than stem bark to microorganisms namely Staphylococcus aureus, Corynebacterium minutissimum, and Streptococcus spp. Sensitivity of trunk bark can be attributed to a more developed phytoconstituents. Dermal sensitization test on both sexes of rabbits using the following concentrations: 100%, 40% and 20% of extract showed that Tamarind has no irritating property and therefore safe for formulation into an antibacterial cream. Excipients used for formulation such as methyl paraben, propyl paraben, stearyl alcohol and white petrolatum were compatible with the Tamarind acetone extract through Differential Scanning Calorimetry except sodium lauryl sulfate that exhibited crystallization when subjected at 200˚C. The method of manufacture used in cream is fusion, therefore strict compliance of processing temperature should be observed to prevent polymorphism. Quality control tests of formulated cream based on USP 30 and Philippine Pharmacopeia were satisfactory.

Keywords: antibacterial, differential scanning calorimetry, tannins, dermal sensitization

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Authors: Rohit Singh Dangi, Ravi Kant Pal, Monica Sundd

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Acyl-CoA binding protein (ACBP) is a housekeeping protein which functions as an intracellular carrier of acyl-CoA esters. Given the fact that the amastigote stage (blood stage) of Leishmania depends largely on fatty acids as the energy source, of which a large part is derived from its host, these proteins might have an important role in its survival. In Leishmania major, genome sequencing suggests the presence of six ACBPs, whose function remains largely unknown. For functional and structural characterization, one of the ACBP genes was cloned, and the protein was expressed and purified heterologously. Acyl-CoA ester binding and stoichiometry were analyzed by isothermal titration calorimetry and Dynamic light scattering. Our results shed light on high affinity of ACBP towards longer acyl-CoA esters, such as myristoyl-CoA to arachidonoyl-CoA with single binding site. To understand the binding mechanism & dynamics, Nuclear magnetic resonance assignments of this protein are being done. The protein's crystal structure was determined at 1.5Å resolution and revealed a classical topology for ACBP, containing four alpha-helical bundles. In the binding pocket, the loop between the first and the second helix (16 – 26AA) is four residues longer from other extensively studied ACBPs (PfACBP) and it curls upwards towards the pantothenate moiety of CoA to provide a large tunnel space for long acyl chain insertion.

Keywords: acyl-coa binding protein (ACBP), acyl-coa esters, crystal structure, isothermal titration, calorimetry, Leishmania

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Authors: Gabriel K. Nzulu, Lina Rostorm, Hans Högberg, Jun Liu, per Eklund, Lars Hultman, Martin Magnuson

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Altered and gangue quartz in hydrothermal veins from the Kubi Gold deposit in Dunkwa on Offin in the central region of Ghana are investigated for possible Au associated pathfinder minerals and to provide understanding and increase the knowledge of the mineral hosting and alteration processes in quartz. X-ray diffraction, air annealing furnace, differential scanning calorimetry, energy dispersive X-ray spectroscopy, and transmission electron microscopy have been applied on different quartz types outcropping from surface and bed rocks at the Kubi Gold Mining to reveal the material properties at different temperatures. From the diffraction results of the fresh and annealed quartz samples, we find that the samples contain pathfinder and the impurity minerals FeS₂, biotite, TiO₂, and magnetite. These minerals, under oxidation process between 574-1400 °C temperatures experienced hematite alterations and a transformation from α-quartz to β-quartz and further to cristobalite as observed from the calorimetry scans for hydrothermally exposed materials. The energy dispersive spectroscopy revealed elemental species of Fe, S, Mg, K, Al, Ti, Na, Si, O, and Ca contained in the samples and these are attributed to the impurity phase minerals observed in the diffraction. The findings also suggest that during the hydrothermal flow regime, impurity minerals and metals can be trapped by voids and faults. Under favorable temperature conditions the trapped minerals can be altered to change color at different depositional stages by oxidation and reduction processes leading to hematite alteration which is a useful pathfinder in mineral exploration.

Keywords: quartz, hydrothermal, minerals, hematite, x-ray diffraction, crystal-structure, defects

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Authors: M. Khlifa, A. Youssef, A. F. Zaed, A. Kraft, V. Arrighi

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A series of PS-nanoparticles were prepared by grafting PS from both aggregated silica and colloidally silica using atom-transfer radical polymerisation (ATRP). The mechanical behaviour of the nanocomposites have been examined by differential scanning calorimetry (DSC)and dynamic mechanical thermal analysis (DMTA).

Keywords: ATRP, nanocomposites, polystyrene, reinforcement

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Authors: Ekere E. Kokonne, Isimi C. Yetunde, Okoh E. Judith, Okafor E. Ijeoma, Ajeh J. Isaac, Olobayo O. Kunle, Emeje O. Martins

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NIPRIMAL® is a mono herbal formulation of Nauclea latifolia used in the treatment of malaria. The stability of extracts made from plant material is essential to ensure the quality, safety and efficacy of the finished product. This study assessed the stability of the formulation under three different storage conditions; normal room temperature, infrared and under refrigeration. Differential Scanning Calorimetry (DSC) and Thin Layer Chromatography (TLC) were used to monitor the formulations. The DSC analysis was done from 0oC to 350oC under the three storage conditions. Results obtained indicate that NIPRIMAL® was stable at all the storage conditions investigated. Thin layer chromatography (TLC) after 6 months showed there was no significant difference between retention factor (RF) values for the various storage conditions. The reference sample had four spots with RF values of 0.47, 0.68, 0.76, 0.82 respectively and these spots were retained in the test formulations with corresponding RF values were after 6 months at room temperature and refrigerated temperature been 0.56, 0.73, 0.80, 0.92 and 0.47, 0.68, 0.76, 0.82 respectively. On the other hand, the RF values (0.55, 0.74, 0.77, 0.93) obtained under infrared after 1 month varied slightly from the reference. The sample exposed to infrared had a lower heat capacity compared to that stored under room temperature or refrigeration. A combination of TLC and DSC measurements has been applied for assessing the stability of NIPRIMAL®. Both methods were found to be rapid, sensitive and reliable in determining its stability. It is concluded that NIPRIMAL® can be stored under any of the tested conditions without degradation. This study is a major contribution towards developing appropriate stability monitoring parameters for herbal products.

Keywords: differential scanning calorimetry, formulation, NIPRIMAL®, stability, thin layer hromatography

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Authors: Hong-Min Kim, Da-Som Han, Myong-Hoon Lee

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CLCs (Cholesteric liquid crystals) draw tremendous interest due to their potential in various applications such as cholesteric color filters in LCD devices. CLC possesses helical molecular orientation which is induced by a chiral dopant molecules mixed with nematic liquid crystals. The efficiency of a chiral dopant is quantified by the HTP (helical twisting power). In this work, we designed and synthesized a series of new chiral dopants having a Schiff’s base imine structure with different alkyl chain lengths (butyl, hexyl and octyl) from chiral naphthyl amine by two-step reaction. The structures of new chiral dopants were confirmed by 1H-NMR and IR spectroscopy. The properties were investigated by DSC (differential scanning calorimetry calorimetry), POM (polarized optical microscopy) and UV-Vis spectrophotometer. These solid state chiral dopants showed excellent solubility in nematic LC (MLC-6845-000) higher than 17wt%. We prepared the CLC(Cholesteric Liquid Crystal) cell by mixing nematic LC (MLC-6845-000) with different concentrations of chiral dopants and injecting into the sandwich cell of 5μm cell gap with antiparallel alignment. The cholesteric liquid crystal phase was confirmed from POM, in which all the samples showed planar phase, a typical phase of the cholesteric liquid crystals. The HTP (helical twisting power) is one of the most important properties of CLC. We measured the HTP values from the UV-Vis transmittance spectra of CLC cells with varies chiral dopant concentration. The HTP values with different alkyl chains are as follows: butyl chiral dopant=29.8μm-1; hexyl chiral dopant= 31.8μm-1; octyl chiral dopant=27.7μm-1. We obtained the red, green and blue reflection color from CLC cells, which can be used as color filters in LCDs applications.

Keywords: cholesteric liquid crystal, color filter, display, HTP

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: Matthew Korey, Jeffrey Youngblood, John Howarter

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Background and Significance: Tannic acid (TA) is a bio-based high molecular weight organic, aromatic molecule that has been found to increase thermal stability and flame retardancy of many polymer matrices when used as an additive. Although it is biologically sourced, TA is a pollutant in industrial wastewater streams, and there is a desire to find applications in which to downcycle this molecule after extraction from these streams. Additionally, epoxy thermosets have revolutionized many industries, but are too flammable to be used in many applications without additives which augment their flame retardancy (FR). Many flame retardants used in epoxy thermosets are synthesized from petroleum-based monomers leading to significant environmental impacts on the industrial scale. Many of these compounds also have significant impacts on human health. Various bio-based modifiers have been developed to improve the FR of the epoxy resin; however, increasing FR of the system without tradeoffs with other properties has proven challenging, especially for TA. Methodologies: In this work, TA was incorporated into the thermoset by use of solvent-exchange using methyl ethyl ketone, a co-solvent for TA, and epoxy resin. Samples were then characterized optically (UV-vis spectroscopy and optical microscopy), thermally (thermogravimetric analysis and differential scanning calorimetry), and for their flame retardancy (mass loss calorimetry). Major Findings: Compared to control samples, all samples were found to have increased thermal stability. Further, the addition of tannic acid to the polymer matrix by the use of solvent greatly increased the compatibility of the additive in epoxy thermosets. By using solvent-exchange, the highest loading level of TA found in literature was achieved in this work (40 wt%). Conclusions: The use of solvent-exchange shows promises for circumventing the limitations of TA in epoxy.

Keywords: sustainable, flame retardant, epoxy, tannic acid

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Authors: M. Fatmi, T. Chihi, M. A. Ghebouli, B. Ghebouli

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This work presents the experimental results of the differential scanning calorimetry (DSC), hardness measurements (Hv) and XRD analysis, for order to investigate the kinetics of precipitation phenomena in Al-7%wt. Mg alloy. In the XRD and DSC curves indicates the formation of the intermediate precipitation of β-(Al3Mg2) phase respectively. The activation energies associated with the processes have been determined according to the three models proposed by Kissinger, Ozawa, and Boswell. Consequently, the nucleation mechanism of the precipitates can be explained. These phases are confirmed by XRD analysis.

Keywords: discontinuous precipitation, hardening, Al–Mg alloys, mechanical and mechatronics engineering

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Authors: Patricia Mikchaela D. L. Feliciano, Ciela Kadeshka A. Fuentes, Bea Trixia B. Gales, Ethel Princess A. Gepulango, Martin R. Hernandez, Elina Andrea S. Lantion, Jhoe Cynder P. Legaspi, Peter F. Quilala, Gina C. Castro

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Propolis is a resin-like material used by bees to fill large gap holes in the beehive. It has been found to possess anti-inflammatory property, which stimulates hair growth in rats by inducing hair keratinocytes proliferation, causing water retention and preventing damage caused by heat, ultraviolet rays, and other microorganisms without abnormalities in hair follicles. The present study aimed to formulate 10% and 30% Propolis Hair Cream for use in enhancing hair properties. Raw propolis sample was tested for heavy metals using Atomic Absorption Spectroscopy; zinc and chromium were found to be present. Likewise, propolis was extracted in a percolator using 70% ethanol and concentrated under vacuum using a rotary evaporator. The propolis extract was analyzed for total flavonoid content. Compatibility of the propolis extract with excipients was evaluated using Differential Scanning Calorimetry (DSC). No significant changes in organoleptic properties, pH and viscosity of the formulated creams were noted after four weeks of storage at 2-8°C, 30°C, and 40°C. The formulated creams were found to be non-irritating based on the Modified Draize Rabbit Test. In vivo efficacy was evaluated based on thickness and tensile strength of hair grown on previously shaved rat skin. Results show that the formulated 30% propolis-based cream had greater hair enhancing properties than the 10% propolis cream, which had a comparable effect with minoxidil.

Keywords: atomic absorption spectroscopy, differential scanning calorimetry (DSC), modified draize rabbit test, propolis

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Authors: Rishi Sharma, S. N. Maiti

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The non-isothermal crystallization kinetics of PP/SEBS-g-MA blends up to 0-50% concentration of copolymer was studied by differential scanning calorimetry at four different cooling rates. Crystallization parameters were analyzed by Avrami and Jeziorny models. Primary and secondary crystallization processes were described by Avrami equation. Avrami model showed that all types of shapes grow from small dimensions during primary crystallization. However, three-dimensional crystal growth was observed during the secondary crystallization process. The crystallization peak and onset temperature decrease, however

Keywords: crystallization kinetics, non-isothermal, polypropylene, SEBS-g-MA

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Authors: I. Belyamani, M. K. Hassan, J. U. Otaigbe, W. R. Fielding, K. A. Mauritz, J. S. Wiggins, W. L. Jarrett

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We have investigated the flame-retardant efficiency of special new phosphate glass (P-glass) compositions having different glass transition temperatures (Tg) on the processing conditions of polyamide 6,6 (PA6,6) and the final hybrid flame retardancy (FR). We have showed that the low Tg P glass composition (i.e., ILT 1) is a promising flame retardant for PA6,6 at a concentration of up to 15 wt. % compared to intermediate (IIT 3) and high (IHT 1) Tg P glasses. Cone calorimetry data showed that the ILT 1 decreased both the peak heat release rate and the total heat amount released from the PA6,6/ILT 1 hybrids, resulting in an efficient formation of a glassy char layer. These intriguing findings prompted to address several questions concerning the mechanism of action of the different P glasses studied. The general mechanism of action of phosphorous based FR additives occurs during the combustion stage by enhancing the morphology of the char and the thermal shielding effect. However, the present work shows that P glass based FR additives act during melt processing of PA6,6/P glass hybrids. Dynamic mechanical analysis (DMA) revealed that the Tg of PA6,6/ILT 1 was significantly shifted to a lower Tg (~65 oC) and another transition appeared at high temperature (~ 166 oC), thus indicating a strong interaction between PA6,6 and ILT 1. This was supported by a drop in the melting point and crystallinity of the PA6,6/ILT 1 hybrid material as detected by differential scanning calorimetry (DSC). The dielectric spectroscopic investigation of the networks’ molecular level structural variations (i.e. hybrids chain motion, Tg and sub-Tg relaxations) agreed very well with the DMA and DSC findings; it was found that the three different P glass compositions did not show any effect on the PA6,6 sub-Tg relaxations (related to the NH2 and OH chain end groups motions). Nevertheless, contrary to IIT 3 and IHT 1 based hybrids, the PA6,6/ILT 1 hybrid material showed an evidence of splitting the PA6,6 Tg relaxations into two peaks. Finally, the CPMAS 31P-NMR data confirmed the miscibility between ILT 1 and PA6,6 at the molecular level, as a much larger enhancement in cross-polarization for the PA6,6/15%ILT 1 hybrids was observed. It can be concluded that compounding low Tg P-glass (i.e. ILT 1) with PA6,6 facilitates hydrolytic chain scission of the PA6,6 macromolecules through a potential chemical interaction between phosphate and the alpha-Carbon of the amide bonds of the PA6,6, leading to better flame retardant properties.

Keywords: broadband dielectric spectroscopy, composites, flame retardant, polyamide, phosphate glass, sustainable

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Authors: C. Amrane, D. Haman

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Aluminum-magnesium alloys are widely used in industry thanks to their mechanical properties and corrosion resistivity. These properties are related to the magnesium content and to the applied heat treatments. Although they are already well studied, questions concerning the microstructural stability and the effect of different heat treatments are still being asked. In this work we have presented a comparative study on the behavior of the precipitation reactions during different heat treatment in two different Al-Mg alloys (Al–8 wt. % Mg and Al–12 wt. % Mg). For this purpose, we have used various experimental techniques as dilatometry, calorimetry, optical microscopy, and microhardness measurements. The obtained results shown that, the precipitation kinetics and the mechanical responses to the applied heat treatments, of the two studied alloys, are different.

Keywords: Al-Mg alloys, precipitation, hardness, heat treatments

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Authors: Karina I. Hidas, Csaba Németh, Anna Visy, Judit Csonka, László Friedrich, Ildikó Cs. Nyulas-Zeke

Abstract:

Egg yolk is a popular ingredient in the food industry due to its gelling, emulsifying, colouring, and coagulating properties. Because of the heat sensitivity of proteins, egg yolk can only be heat treated at low temperatures, so its shelf life, even with the addition of a preservative, is only a few weeks. Freezing can increase the shelf life of liquid egg yolk up to 1 year, but it undergoes gelling below -6 ° C, which is an irreversible phenomenon. The degree of gelation depends on the time and temperature of freezing and is influenced by the process of thawing. Therefore, in our experiment, we examined egg yolks thawed in different ways. In this study, unpasteurized, industrially broken, separated, and homogenized liquid egg yolk was used. Freshly produced samples were frozen in plastic containers at -18°C in a laboratory freezer. Frozen storage was performed for 90 days. Samples were analysed at day zero (unfrozen) and after frozen storage for 1, 7, 14, 30, 60 and 90 days. Samples were thawed in two ways (at 5°C for 24 hours and 30°C for 3 hours) before testing. Calorimetric properties were examined by differential scanning calorimetry, where heat flow curves were recorded. Denaturation enthalpy values were calculated by fitting a linear baseline, and denaturation temperature values were evaluated. Besides, dry matter content of samples was measured by the oven method with drying at 105°C to constant weight. For statistical analysis two-way ANOVA (α = 0.05) was employed, where thawing mode and freezing time were the fixed factors. Denaturation enthalpy values decreased from 1.1 to 0.47 at the end of the storage experiment, which represents a reduction of about 60%. The effect of freezing time was significant on these values, already the enthalpy of samples stored frozen for 1 day was significantly reduced. However, the mode of thawing did not significantly affect the denaturation enthalpy of the samples, and no interaction was seen between the two factors. The denaturation temperature and dry matter content did not change significantly either during the freezing period or during the defrosting mode. Results of our study show that slow freezing and frozen storage at -18°C greatly reduces the amount of protein that can be denatured in egg yolk, indicating that the proteins have been subjected to aggregation, denaturation or other protein conversions regardless of how they were thawed.

Keywords: denaturation enthalpy, differential scanning calorimetry, liquid egg yolk, slow freezing

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Authors: Kwangin Kim, Taewon Yoo, Haksoo Han

Abstract:

Polyimide is a superior polymer in the electronics industry, and we conducted a study to synthesize poly(amide-imide) at low temperatures. Poly(amide-imide) was synthesized at low-temperature curing to offer a thermal stable membrane with low residual stress and good processability. As a result, the low crack polymer with good processability could be used to various applications such as semiconductors, integrated circuits, coating materials, membranes, and display. The synthesis of poly(amide-imide) at low temperatures was confirmed by Fourier transform infrared spectroscopy (FT-IR). Thermal stabilities of the polymer was confirmed by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC).

Keywords: poly(amide-imide), residual stress, thermal stability

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Authors: H. A. Brandão Cordeiro, M. G. Bocardo, N. C. Penteado, V. T. de Moraes, S. M. Giampietri Lebrão, G. W. Lebrão

Abstract:

The present study desired to obtain a nanocomposite of epoxy resin reinforced with graphene oxide (OG), for aerospace application, produced by aqueous emulsion. It was obtained proof bodies with 0.00 wt%, 0.10 wt%, 0.25 wt% and 0.50 wt% in weight of nanoparticles, to check the influence of it in the final quality of the obtained product. The validation of the results was done by the application thermal characterization by differential scanning calorimetry (DSC). It was seen that the nanocomposite reinforced with 0.10 wt% of OG showed the best results, the average glass transition temperature, at 2 °C, compared to the pure resin.

Keywords: aqueous emulsion, graphene, nanocomposites, thermal characterization

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Authors: A. de Folly d’Auris, R. Bagatin, P. Filtri

Abstract:

This paper discusses the importance of having a good initial characterization of soil samples when thermal desorption has to be applied to polluted soils for the removal of contaminants. Particular attention has to be devoted on the desorption kinetics of the samples to identify the gases evolved during the heating, and contaminant degradation pathways. In this study, two samples coming from different points of the same contaminated site were considered. The samples are much different from each other. Moreover, the presence of high initial quantity of heavy hydrocarbons strongly affected the performance of thermal desorption, resulting in formation of dangerous intermediates. Analytical techniques such TGA (Thermogravimetric Analysis), DSC (Differential Scanning Calorimetry) and GC-MS (Gas Chromatography-Mass) provided a good support to give correct indication for field application.

Keywords: desorption kinetics, hydrocarbons, thermal desorption, thermogravimetric measurements

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Authors: A. Azizi, M. Toubane, L. Chetibi

Abstract:

Differential scanning calorimetry (DSC) is a widely used technique for the study of phase transformations, particularly in the study of precipitation. The kinetic of the precipitation and dissolution is always related to the concept of activation energy Ea. The determination of the activation energy gives important information about the kinetic of the precipitation reaction. In this work, we were interested in the study of the isothermal and non-isothermal treatments on the decomposition of the supersaturated solid solution in the alloy AZ91 (Mg-9 Al-Zn 1-0.2 Mn. mass fraction %), using Differential Calorimetric method. Through this method, the samples were heat treated up to 425° C, using different rates. To calculate the apparent activation energies associated with the formation of precipitated phases, we used different isoconversional methods. This study was supported by other analysis: X-ray diffraction and microhardness measurements.

Keywords: calorimetric, activation energy, AZ91 alloys, microstructural evolution

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Authors: M. Boháč, R. Novotný, F. Frajkorová, R. S. Yadav, T. Opravil, M. Palou

Abstract:

Properties of Portland cement mixtures with various fractions of metakaolin were studied. 10 % of Portland cement CEM I 42.5 R was replaced by different fractions of high reactivity metakaolin with defined chemical and mineralogical properties. Various fractions of metakaolin were prepared by jet mill classifying system. There is a clear trend between fineness of metakaolin and hydration heat development. Due to metakaolin presence in mixtures the compressive strength development of mortars is rather slower for coarser fractions but 28-day flexural strengths are improved for all fractions of metakaoline used in mixtures compared to reference sample of pure Portland cement. Yield point, plastic viscosity and adhesion of fresh pastes are considerably influenced by fineness of metakaolin used in cement pastes.

Keywords: calorimetry, cement, metakaolin fineness, rheology, strength

Procedia PDF Downloads 378