Abstract: Propellants based on Hydroxyl Terminated Polybutadiene/Ammonium Perchlorate (HTPB/AP) are the most commonly used in most of the rocket engines used by the Brazilian Armed Forces. This work aimed at the possibility of extending its useful life (currently in 10 years) by performing kinetic-chemical analyzes of its energetic material via Differential Scanning Calorimetry (DSC) and also performing computer simulation of aging process using the software Large-scale Atomic/Molecular Massively Parallel Simulator (LAMMPS). Thermal analysis via DSC was performed in triplicates and in three heating ratios (5 ºC, 10 ºC, and 15 ºC) of rocket motor with 11 years shelf-life, using the Arrhenius equation to obtain its activation energy, using Ozawa and Kissinger kinetic methods, allowing comparison with manufacturing period data (standard motor). In addition, the kinetic parameters of internal pressure of the combustion chamber in 08 rocket engines with 11 years of shelf-life were also acquired, for comparison purposes with the engine start-up data.
Abstract: As composite materials continue to gain popularity in the aerospace industry; large airframe sections made out of composite materials are becoming the standard for aerospace manufacturers. However, the heavy utilization of these composite materials also increases the importance of the recycling of these composite materials. A team of Purdue University School of Aviation and Transportation Technology (SATT) faculty and students have partnered to investigate the characteristics of 3D printed recycled carbon fiber. A prototype of a 3D printed recycled carbon fiber part was provided by an industry partner and different sections of the prototype were used to create specimens. A furnace was utilized in order to remove the polymer from the specimens and the specimen’s fiber content and fiber length was calculated from the remaining fibers. A differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) test was also conducted on the 3D printed recycled carbon fiber prototype in order to determine the prototype’s degree of cure at different locations. The data collected from this study provided valuable information in the process improvement and understanding of 3D printed recycled carbon fiber.
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.
Abstract: Two organic dyes comprising carbazole as the electron donors and cyanoacetic acid moieties as the electron acceptors were synthesized. The organic dye was prepared by standard reaction from carbazole as the starting material. To this end, carbazole was reacted with bromobenzene and further oxidation and reacted with cyanoacetic acid. The obtained organic dye was purified and characterized using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance (1HNMR), carbon nuclear magnetic resonance (13CNMR) and elemental analysis. The influence of heteroatom on carbazole donors and cyno substitution on the acid acceptor is evidenced by spectral and electrochemical photovoltaic experiments. Finally, light fastness properties for organic dye were investigated.
Abstract: Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.
Abstract: The structure-property relationship and initiator effect on bulk polymerized poly(methyl methacrylate) (PMMA)–oragnomodified layered silicate nanocomposites was investigated. In this study, we used 2, 2'-azobis (4-methoxy-2,4-dimethyl valeronitrile and benzoyl peroxide initiators for bulk polymerization. The bulk polymerized nanocomposites’ morphology was investigated by X-ray diffraction and transmission electron microscopy. The type of initiator strongly influences the physiochemical properties of the polymer nanocomposite. The thermal degradation of PMMA in the presence of nanofiller was studied. 5 wt% weight loss temperature (T5d) increased as compared to pure PMMA. The peak degradation temperature increased for the nanocomposites. Differential scanning calorimetry and dynamic mechanical analysis were performed to investigate the glass transition temperature and the nature of the constrained region as the reinforcement mechanism respectively. Furthermore, the optical properties such as UV-Vis and Total Luminous Transmission of nanocomposites are examined.
Abstract: Environmental and sustainability concerns push the industries to manufacture alternative materials having less environmental impact. The Wood Plastic Composites (WPCs) produced by blending the biopolymers and natural fillers permit not only to tailor the desired properties of materials but also are the solution to meet the environmental and sustainability requirements. This work presents the elaboration and characterization of the fully green WPCs prepared by blending a biopolymer, BIOPLAST® GS 2189 and spruce sawdust used as filler with different amounts. Since both components are bio-based, the resulting material is entirely environmentally friendly. The mechanical, thermal, structural properties of these WPCs were characterized by different analytical methods like tensile, flexural and impact tests, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and X-ray Diffraction (XRD). Their water absorption properties and resistance to the termite and fungal attacks were determined in relation with different wood filler content. The tensile and flexural moduli of WPCs increased with increasing amount of wood fillers into the biopolymer, but WPCs became more brittle compared to the neat polymer. Incorporation of spruce sawdust modified the thermal properties of polymer: The degradation, cold crystallization, and melting temperatures shifted to higher temperatures when spruce sawdust was added into polymer. The termite, fungal and water absorption resistance of WPCs decreased with increasing wood amount in WPCs, but remained in durability class 1 (durable) concerning fungal resistance and quoted 1 (attempted attack) in visual rating regarding to the termites resistance except that the WPC with the highest wood content (30 wt%) rated 2 (slight attack) indicating a long term durability. All the results showed the possibility to elaborate the easy injectable composite materials with adjustable properties by incorporation of BIOPLAST® GS 2189 and spruce sawdust. Therefore, lightweight WPCs allow both to recycle wood industry byproducts and to produce a full ecologic material.
Abstract: Cellulose acetate (CA) is a natural biodegradable polymer. It forms transparent films by the casting technique. CA suffers from high degree of water permeability as well as the low thermal stability at high temperatures. To adjust the CA polymeric films to the manufacture of food packaging, its thermal and mechanical properties should be improved. The modification of CA by grafting it with N-Amino phenyl maleimide (N-APhM) led to the construction of hydrophobic branches throughout the polymeric matrix which reduced its wettability as compared to the parent CA. The branches built onto the polymeric chains had been characterized by UV/Vis, 13C-NMR and ESEM. The improvement of the thermal properties was investigated and compared to the parent CA using thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), differential thermal analysis (DTA), contact angle and mechanical testing measurements. The results revealed that the water-uptake was reduced by increasing the graft percentage. The thermal and mechanical properties were also improved.
Abstract: Polymer based membranes are one of the low-cost technologies available for the gas separation. Three major elements required for a commercial gas separating membrane are high permeability, high selectivity, and good mechanical strength. Poly(vinylidene fluoride) (PVDF) is a commercially available fluoropolymer and a widely used membrane material in gas separation devices since it possesses remarkable thermal, chemical stability, and excellent mechanical strength. The PVDF membrane was chemically modified by soaking in different ionic liquids and dried. The thermal behavior of modified membranes was investigated by differential scanning calorimetry (DSC), and thermogravimetry (TGA), and the results clearly show the best affinity between the ionic liquid and the polymer support. The porous structure of the PVDF membranes was clearly seen in the scanning electron microscopy (SEM) images. The CO₂ permeability of blended membranes was explored in comparison with the unmodified matrix. The ionic liquid immobilized in the hydrophobic PVDF support exhibited good performance for separations of CO₂/N₂. The improved permeability of modified membrane (PVDF-IL) is attributed to the high concentration of nitrogen rich imidazolium moieties.
Abstract: In this study, a form-stable composite Paraffin/Nanoclay (PA-NC) has been prepared by absorbing PA into porous particles of NC to be used for low-temperature latent heat thermal energy storage. The leakage test shows that the maximum mass fraction of PA that can be incorporated in NC without leakage is 60 wt.%. Differential scanning calorimetry (DSC) has been used to measure the thermal properties of the PA and PA-NC both before and after incorporation in plasterboard (PL). The mechanical performance of the samples has been evaluated in flexural mode. The thermal energy storage performance has been studied using a small test chamber (100 mm × 100 mm × 100 mm) made from 10 mm thick PL and measuring the temperatures using thermocouples. The flammability of the PL+PL-NC has been discussed using a cone calorimeter. The results indicate that the form composite PA has good potential for use as thermal energy storage materials in building applications.
Abstract: Calcined kaolinite clay (CKC) is a pozzolanic material that is current drawing research attention. This work investigates the conditions for the best performance of a CKC from a kaolinite clay source in Ajebo, Abeokuta (southwest Nigeria) known for its commercial availability. Samples from this source were subjected to X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). XRD shows that kaolinite is the main mineral in the clay source. This mineral is responsible for the pozzolanic behavior of CKC. DSC indicates that the transformation from the clay to CKC occurred between 550 and 750 oC. Using this temperature range, clay samples were milled and different CKC samples were produced in an electric muffle furnace using temperatures of 550, 600, 650, 700, 750 and 800 oC respectively for 1 hour each. This was also repeated for 2 hours. The degree of de-hydroxylation (dtg) and strength activity index (SAI) were also determined for each of the CKC samples. The dtg and SAI tests were repeated two more times for each sample and averages were taken. Results showed that peak dtg occurred at 750 oC for 1 hour calcining combination (94.27%) whereas marginal differences were recorded at some lower temperatures (90.97% for 650 oC for 2 hours; 91.05% for 700 oC for 1 hour and 92.77% for 700 oC for 2 hours). Optimum SAI was reported at 700 oC for 1 hour (99.05%). Rating SAI as a better parameter than dtg, 700 oC for 1 hour combination was adopted as the best calcining condition. The paper recommends the adoption of this clay source for pozzolan production by adopting the calcining conditions established in this work.
Abstract: Cefixime, a BCS class II drug, is insoluble in water but freely soluble in acetone and in alcohol. The aqueous solubility of cefixime in water is poor and exhibits exceptionally slow and intrinsic dissolution rate. In the present study, cefixime and β-Cyclodextrin (β-CD) solid dispersions were prepared with a view to study the effect and influence of β-CD on the solubility and dissolution rate of this poorly aqueous soluble drug. Phase solubility profile revealed that the solubility of cefixime was increased in the presence of β-CD and was classified as AL-type. Effect of variable, such as drug:carrier ratio, was studied. Physical characterization of the solid dispersion was characterized by Fourier transform infrared spectroscopy (FT-IR) and Differential scanning calorimetry (DSC). These studies revealed that a distinct loss of drug crystallinity in the solid molecular dispersions is ostensibly accounting for enhancement of dissolution rate in distilled water. The drug release from the prepared solid dispersion exhibited a first order kinetics. Solid dispersions of cefixime showed a 6.77 times fold increase in dissolution rate over the pure drug.
Abstract: In the last few decades, due to their advanced properties, there has been an increasing interest in hybrid composite materials. In this study, the effect of different stacking sequences of jute and carbon fabric plies on dynamic mechanical properties of composite laminates were investigated. Vacuum bagging system was used to fabricate the composite samples. Each composite laminate was reinforced with two plies of jute fabric and two plies of carbon fabric by varying the position of layers. Dynamic mechanical analyzer (DMA) was used to examine the dynamic mechanical properties of composite laminates with increasing temperature. Results showed that the composite sample, which has carbon fabric at the outer layers, has the highest storage and loss modulus. Besides, it was observed that glass transition temperature (Tg) of samples are close to each other and at about 75 °C.
Abstract: Sorghum byproducts, namely bran, stalk, and panicle are examples of lignocellulosic biomass. These raw materials contain large amounts of polysaccharides, in particular hemicelluloses, celluloses, and lignins, which if efficiently extracted, can be utilised for the development of a range of added value products with potential applications in agriculture and food packaging sectors. The aim of this study was to characterise fractions extracted from sorghum bran and stalk with regards to their physicochemical properties that could determine their applicability as food-packaging materials. A sequential alkaline extraction was applied for the isolation of cellulosic, hemicellulosic and lignin fractions from sorghum stalk and bran. Lignin content, phenolic content and antioxidant capacity were also investigated in the case of the lignin fraction. Thermal analysis using differential scanning calorimetry (DSC) and X-Ray Diffraction (XRD) revealed that the glass transition temperature (Tg) of cellulose fraction of the stalk was ~78.33 oC at amorphous state (~65%) and water content of ~5%. In terms of hemicellulose, the Tg value of stalk was slightly lower compared to bran at amorphous state (~54%) and had less water content (~2%). It is evident that hemicelluloses generally showed a lower thermal stability compared to cellulose, probably due to their lack of crystallinity. Additionally, bran had higher arabinose-to-xylose ratio (0.82) than the stalk, a fact that indicated its low crystallinity. Furthermore, lignin fraction had Tg value of ~93 oC at amorphous state (~11%). Stalk-derived lignin fraction contained more phenolic compounds (mainly consisting of p-coumaric and ferulic acid) and had higher lignin content and antioxidant capacity compared to bran-derived lignin fraction.
Abstract: In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)4 to titanium oxide, TiO2 was investigated. The as-prepared Ti(OH)4 precipitate was annealed at 800°C to obtain TiO2 nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO2 nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO2 nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.
Abstract: This work involves the degradation of plastic waste in the presence of three different nanocatalysts. A thin film of LLDPE was formed with all three nanocatalysts separately in the solvent. Thermo Gravimetric Analysis (TGA) and Differential Scanning Calorimetric (DSC) analysis of polymers suggest that the presence of these catalysts lowers the degradation temperature and the change mechanism of degradation. Gas chromatographic analysis was carried out for two films. In gas chromatography (GC) analysis, it was found that degradation of pure polymer produces only 32% C3/C4 hydrocarbons and 67.6% C5/C9 hydrocarbons. In the presence of these catalysts, more than 80% of polymer by weight was converted into either liquid or gaseous hydrocarbons. Change in the mechanism of degradation of polymer was observed therefore more C3/C4 hydrocarbons along with valuable feedstock are produced. Adjustment of dose of nanocatalyst, use of nano-admixtures and recycling of catalyst can make this catalytic feedstock recycling method a good tool to get sustainable environment. The obtained products can be utilized as fuel or can be transformed into other useful products. In accordance with the principles of sustainable development, chemical recycling i.e. tertiary recycling of polymers along with the reuse (zero order recycling) of plastics can be the most appropriate and promising method in this direction. The tertiary recycling is attracting much attention from the viewpoint of the energy resource.
Abstract: A suitable model membrane to study the pharmacological effect of pharmaceutical products is human stratum corneum because this layer of human skin is the outermost layer and it is an important barrier to be passed through. Other model membranes which were also used are for example skins from pig, mouse, reptile or fish. We are interested in fish skins in this project. The advantages of the fish skins are, that they can be obtained from the supermarket or fish shop. However, the fish skins should be freshly prepared and used directly without storage. In order to understand the effect of different model drugs e.g. lidocaine HCl, resveratrol, paracetamol, ibuprofen, acetyl salicylic acid on the properties of the model membrane from various types of fishes e.g. trout, salmon, cod, plaice permeation tests were performed and differential scanning calorimetry was applied.
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.
Abstract: 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.
Abstract: Some of the main causes for degradation of polymeric materials are thermal aging, hydrolysis, oxidation or chemical degradation by acids, alkalis or water. The first part of this paper provides a brief summary of advances in technology, methods and specification of composite materials for relining as a rehabilitation technique for sewage systems. The second part summarizes an investigation on frequently used composite materials for relining in Sweden, the rubber filled epoxy composite and reinforced polyester composite when they were immersed in deionized water or in dry conditions, and elevated temperatures up to 80°C in the laboratory. The tests were conducted by visual inspection, microscopy, Dynamic Mechanical Analysis (DMA), Differential Scanning Calorimetry (DSC) as well as mechanical testing, three point bending and tensile testing.