The properties of fibre-reinforced composites are dependent not only on the strength of the reinforcementfibre but also on the distribution of fibre strength and the composition of the chemicals or additivesaddition within the composites. In this study, the tensile properties of abaca fibre reinforced high impactpolystyrene (HIPS) composites, which had been produced with the parameters of fibre loading (30,40,50wt.%), coupling agent maleic anhydride (MAH) (1,2,3 wt%) and impact modifier (4,5,6 wt.%) weremeasured. The optimum amount of MAH is 3% and the impact modifier is 6% and these give the besttensile properties. Meanwhile, Differential Scanning Calorimetry (DSC) was used to study the thermalbehaviour within the optimum conditions of the composites. In this research, glass transitions temperature(Tg) of neat HIPS occurred below the Tg of the optimum condition of composites as the temperature ofan amorphous state. The endothermic peak of the composites was in the range of 430-4350C, includingneat HIPS. It was observed that enthalpy of the abaca fibre reinforced HIPS composites yielded belowthe neat HIPS of 748.79 J/g.
Methods of NMR relaxation and differential scanning calorimetry (DSC) were used to study the crystallization of anhydrous milk fat (AMF) obtained from milk and subjected to ultrasonic (US) processing. Amongst the changes in the crystallization nature under the influence of ultrasound are the decrease in the crystallization temperature and the increase in the melting enthalpy of the anhydrous milk fat samples. The increase is ∼30% at 20 min of isothermal crystallization and is presumably explained by the additional formation of β'-form crystals from the melt. The parameters of the Avrami equation applied to the description of experimental data show an increase in the crystallization rate in samples with ultrasonic treatment and a change in the dimension of crystallization with a change in melting temperature.
The objective was to characterize the structural behaviour of indomethacin-cimetidine and naproxen-cimetidine co-amorphous systems (1 : 1 molar ratio) prepared by quench cooling, co-evaporation and ball milling.
The in situ polymorphic forms and thermal transitions of refined, bleached and deodorized palm oil (RBDPO), palm stearin (RBDPS) and palm kernel oil (RBDPKO) were investigated using coupled X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicated that the DSC onset crystallisation temperature of RBDPO was at 22.6°C, with a single reflection at 4.2Å started to appear from 23.4 to 17.1°C, and were followed by two prominent exothermic peaks at 20.1°C and 8.5°C respectively. Further cooling to -40°C leads to the further formation of a β'polymorph. Upon heating, a of β'→βtransformation was observed between 32.1 to 40.8°C, before the sample was completely melted at 43.0°C. The crystallization onset temperature of RBDPS was 44.1°C, with the appearance of the α polymorph at the same temperature as the appearance of the first sharp DSC exothermic peak. This quickly changed from α→β´ in the range 25 to 21.7°C, along with the formation of a small β peak at -40°C. Upon heating, a small XRD peak for the β polymorph was observed between 32.2 to 36.0°C, becoming a mixture of (β´+ β) between 44.0 to 52.5°C. Only the β polymorph survived further heating to 59.8°C. For RBDPKO, the crystallization onset temperature was 11.6°C, with the formation of a single sharp exothermic peak at 6.5°C corresponding to the β' polymorphic form until the temperature reached -40°C. No transformation of the polymorphic form was observed during the melting process of RBDPKO, before being completely melted at 33.2°C. This work has demonstrated the detailed dynamics of polymorphic transformations of PKO and PS, two commercially important hardstocks used widely by industry and will contribute to a greater understanding of their crystallization and melting dynamics.
The adulteration of edible fats is a kind of fraud that impairs the physical and chemical features of the original lipid materials. It has been detected in various food, pharmaceutical and cosmeceutical products. Differential scanning calorimetry (DSC) is the robust thermo-analytical machine that permits to fingerprint the primary crystallisation of triacylglycerols (TAGs) molecules and their transition behaviours. The aims of this study was to assess the cross-contamination caused by lard concentration of 0.5-5% in the mixture systems containing beef tallow (BT) and chicken fat (CF) separately. TAGs species of pure and adulterated lipids in relation to their crystallisation and melting parameters were studied using principal components analysis (PCA). The results showed that by using the heating profiles the discrimination of LD from BT and CF was very clear even at low dose of less than 1%. Same observation was depicted from the crystallisation profiles of BT adulterated by LD doses ranging from 0.1% to 1% and from 2% to 5%, respectively. Furthermore, CF adulterated with LD did not exhibit clear changes on its crystallisation profiles. Consequently, DSC coupled with PCA is one of the techniques that might use to monitor and differentiate the minimum adulteration levels caused by LD in different animal fats.
Cellulose acetate (CA) is an interesting material due to its wide spectrum of utilities across different domains ranging from absorbent to membrane filters. In this study, polystyrene (PS) nanofibres, and cellulose acetate/polystyrene (CA/PS) blend nanofibres with various ratios of CA: PS from 20: 80 to 80: 20 were fabricated by using electrospinning technique. The SEM images show that the nanofibres exhibited non-uniform and random orientation with the average fibre diameter in the range of 100 to 800 nm. It was found that the incorporation of PS had a great effect on the morphology of nanofibre. At high proportion of PS, no or less beaded CA/PS nanofibres were formed. Thermal properties of the composite nanofibres were investigated by using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) techniques. The TGA results showed thermal stability of CA/PS nanofibres were higher than pristine CA.
In this study, dynamic vulcanization process was used to improve the thermal properties of calcium carbonate filled composites. The composites were prepared using a Z-blade mixer at 180oC and rotor speed 50rpm. Thermogravimetric analysis (TGA) and Differential scanning calorimetry (DSC) techniques were used to analyze the thermal properties of the composites. The vulcanized and unvulcanized PP/EPDM composites were filled by CaCO3 at 0, 10, 20, 30, and 40 %wt. Meanwhile, thermogravimetric analysis indicates that the total weight loss of PP/EPDM/CaCO3 composites decreased with increasing filler loading. Dynamic vulcanized composites have higher thermal stability, while the crystallinity of PP/EPDM/CaCO3 composites were increased as compared to unvulcanized composites. Therefore, the thermal properties were improved by the presence of
dynamic vulcanization process.
A chemical modifier (acrylic acid) was used to improve the thermal properties of polypropylene/ ethylene propylene diene terpolymer/calcium carbonate (PP/EPDM/CaCO3) composites. Treated
and untreated PP/EPDM composites were filled by CaCO3 at 0, 20 and 40% wt. The composites
were prepared using Z-blade mixer machine at 180oC and 50 rpm of rotor speed. Thermogravimetric
analysis (TGA) and differential scanning calorimetry (DSC) methods were used to analyze the thermal properties of the composites. Thermogravimetric analysis indicated that the total weight loss of PP/EPDM/CaCO3 composites decreased with the increasing filler loading for the treated and untreated composites. Meanwhile, the presence of acrylic acid was found to have increased the thermal stability and crystallinity of PP/EPDM/CaCO3
.
Knowledge about the thermal and storage behavior of produced protein is important for the purpose of storage, transport and shelve life during industrial application. Recombinant bromelain thermal and storage stability were measured and compared to the commercial bromelain using Differential Scanning Calorimetry (DSC). Recombinant bromelain is more stable than commercial bromelain at higher temperature but the stability was reduced after 7 days of storage at 4oC. Higher energy is needed to break the bond between amino acid chains in recombinant bromelain as shown by the enthalpy obtained, suggesting that recombinant bromelain has good protein structure and conformation compared to commercial.
The effects of food gums addition on wheat dough freeze-thaw and frozen storage stability were studied. Thermal and dynamic mechanical properties of frozen wheat dough without yeast addition were
determined by means of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA).
DSC results revealed that food gums showed the ability to increase freeze-thaw stability in frozen-stored
samples wherein lower difference in melting enthalpy between first and second freeze-thaw cycle was shown. Based on DMA results, in general, difference between Tg’ and storage temperature (- 18°C) of dough became smaller upon addition of food gums. This may have a practical implication whereby the unfrozen phase could be better protected against physical degradation.
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
The melting curves of 11 vegetable oils have been characterised. Vegetable oil samples that were cooled at a constant rate (5 degrees C/min) from the melt showed between one and seven melting endotherms upon heating at four different heating rates (1, 5, 10 and 20 degrees C/min) in a differential scanning calorimeter (DSC). Triacylglycerol (TAG) profiles and iodine value analyses were used to complement the DSC data. Generally, the melting transition temperature shifted to higher values with increased rates of heating. The breadth of the melting endotherm and the area under the melting peak also increased with increasing heating rate. Although the number of endothermic peaks was dependent on heating rate, the melting curves of the oil samples were not straightforward in that there was no correlation between the number of endothermic peaks and heating rates. Multiple melting behaviour in DSC experiments with different heating rates could be explained by: (1) the melting of TAG populations with different melting points; and (2) TAG crystal reorganisation effects. On the basis of the corollary results obtained, vegetable oils and fats may be distinguished from their offset-temperature (Toff) values in the DSC melting curves. The results showed that Toff values of all oil samples were significantly (p < 0.01) different in the melting curves scanned at four different scanning rates. These calorimetric results indicate that DSC is a valuable technique for studying vegetable oils.
The potential of Hylocereus polyrhizus peel (HPP) as a new eco-friendly reinforcement for thermoplastic sago starch/agar composite (TPSS/agar) was investigated. The integration of HPP into TPSS/agar composite aimed to enhance its mechanical and thermal characteristics. The study employed Fourier transform-infrared spectroscopy (FT-IR), Scanning electron microscopy (SEM), Thermogravimetric analysis (TGA), and Differential Scanning Calorimetry (DSC), as well as mechanical, physical properties and soil burial testing to analyse the composites. The results showed a favourable miscibility between the matrix and filler, while at higher concentrations of HPP, the starch granules became more visible. The tensile and impact properties of the composites improved significantly after incorporating HPP at 20 wt%, with values of 12.73 MPa and 1.87 kJ/m2, respectively. The glass transition temperature (Tg) and initial decomposition temperature (Ton) decreased with the addition of HPP. The density of the composites reduced from 1.51 ± 0.01 to 1.26 ± 0.01 g/cm3 as the HPP amount increased. The environmental properties indicated that the composites can be composted, with weight loss accelerating from 35 to 60 % and 61 to 91 % by the addition of HPP in 2- and 4-weeks' time, respectively. The study demonstrates the potential of TPSS/agar/HPP composites as eco-friendly materials for various applications.
A synthesis of acrylonitrile (AN)/butyl acrylate (BA)/fumaronitrile (FN) and AN/EHA (ethyl hexyl acrylate)/FN terpolymers was carried out by redox polymerization using sodium bisulfite (SBS) and potassium persulphate (KPS) as initiator at 40 °C. The effect of comonomers, BA and EHA and termonomer, FN on the glass transition temperature (Tg) and stabilization temperature was studied using Differential Scanning Calorimetry (DSC). The degradation behavior and char yield were obtained by Thermogravimetric Analysis. The conversions of AN, comonomers (BA and EHA) and FN were 55%-71%, 85%-91% and 76%-79%, respectively. It was found that with the same comonomer feed (10%), the Tg of AN/EHA copolymer was lower at 63 °C compared to AN/BA copolymer (70 °C). AN/EHA/FN terpolymer also exhibited a lower Tg at 63 °C when compared to that of the AN/BA/FN terpolymer (67 °C). By incorporating BA and EHA into a PAN system, the char yield was reduced to ~38.0% compared to that of AN (~47.7%). It was found that FN reduced the initial cyclization temperature of AN/BA/FN and AN/EHA/FN terpolymers to 228 and 221 °C, respectively, in comparison to that of AN/BA and AN/EHA copolymers (~260 °C). In addition, FN reduced the heat liberation per unit time during the stabilization process that consequently reduced the emission of volatile group during this process. As a result, the char yields of AN/BA/FN and AN/EHA/FN terpolymers are higher at ~45.1% and ~43.9%, respectively, as compared to those of AN/BA copolymer (37.1%) and AN/EHA copolymer (38.0%).
There has been an increasing interest in the use of natural materials as drug delivery vehicles due to their biodegradability, biocompatibility and ready availability. These properties make bacterial cellulose (BC), from nata de coco, a promising biopolymer for drug delivery applications. The aim of this study was to investigate the film-coating and drug release properties of this biopolymer. Physicochemical, morphological and thermal properties of BC films were studied. Model tablets were film coated with BC, using a spray coating technique, and in vitro drug release studies of these tablets were investigated. It was found that BC exhibited excellent ability to form soft, flexible and foldable films without the addition
of any plasticizer. They were comparable to Aquacoat ECD (with plasticizer) in tensile strength, percentage elongation and elasticity modulus. Differential scanning calorimetry (DSC) BC showed a high Tg value indicating thermally stability of films. These results suggest that BC can be used as novel aqueous film-coating agent with lower cost and better film forming properties than existing film-coating agents.
Void-free electrospun SPEEK/Cloisite15A® densed (SP/e-spunCL) membranes are prepared. Different loadings of Cloisite15A® (0.10, 0.15, 0.20, 0.25 and 0.30 wt %) are incorporated into electrospun fibers. The physico-chemical characteristics (methanol permeability, water uptake and proton conductivity) of the membranes are observed. Thermal stability of all membranes is observed using Thermal Gravimetry Analysis (TGA). The thrree stages of degradation range between 163.1 and 613.1 °C. Differential Scanning Calorimetry (DSC) is used to study the wettability of the membranes. SP/e-spunCL15 shows the lowest freezing bound water of 15.27%, which contributed to the lowest methanol permeability. The non-freezing bound water that proportionally increased with proton conductivity of SP/e-spunCL15 membrane is the highest, 10.60%. It is suggested that the electrospinning as the fabricating method has successfully exfoliated the Cloisite in the membrane surface structure, contributing to the decrease of methanol permeability, while the retained water has led to the enhancement of proton conductivity. This new fabrication method of SP/e-spunCL membrane is said to be a desirable polymer electrolyte membrane for future application in direct methanol fuel cell field.
Non-isocyanate polyurethane (NIPU) was prepared from Jatropha curcas oil (JCO) and its alkyd resin via curing with different diamines. The isocyanate-free approach is a green chemistry route, wherein carbon dioxide conversion plays a major role in NIPU preparation. Catalytic carbon dioxide fixation can be achieved through carbonation of epoxidized derivatives of JCO. In this study, 1,3-diaminopropane (DM) and isophorone diamine (IPDA) were used as curing agents separately. Cyclic carbonate conversion was catalyzed by tetrabutylammonium bromide. After epoxy conversion, carbonated JCO (CJCO) and carbonated alkyd resin (CC-AR) with carbonate contents of 24.9 and 20.2 wt %, respectively, were obtained. The molecular weight of CJCO and CC-AR were determined by gel permeation chromatography. JCO carbonates were cured with different amine contents. CJCO was blended with different weight ratios of CC-AR to improve its characteristics. The cured NIPU film was characterized by spectroscopic techniques, differential scanning calorimetry, and a universal testing machine. Field emission scanning electron microscopy was used to analyze the morphology of the NIPU film before and after solvent treatment. The solvent effects on the NIPU film interfacial surface were investigated with water, 30% ethanol, methyl ethyl ketone, 10% HCl, 10% NaCl, and 5% NaOH. NIPU based on CCJO and CC-AR (ratio of 1:3) with IPDA crosslink exhibits high glass transition temperature (44 °C), better solvent and chemical resistance, and Young's modulus (680 MPa) compared with the blend crosslinked with DM. Thus, this study showed that the presence of CC-AR in CJCO-based NIPU can improve the thermomechanical and chemical resistance performance of the NIPU film via a green technology approach.
Polylactic acid (PLA)/Epoxidized natural rubber (ENR-50) blends were prepared by melt extrusion followed by injection
molding to fabricate the test samples. The effect of ENR-50 loadings on the morphological, mechanical, chemical
resistance and water absorption properties of the blends were studied using standard methods. The toughness of the
blend improved with ENR loading up to 20 wt. % but flexural and tensile strength decreased. The balanced mechanical
properties were obtained at 20 wt. % ENR-50 loading. SEM showed good distribution and increased ENR particle size
as ENR content increased from 10 to 30 wt. %. The differential scanning calorimeter (DSC) showed a steady drop in
crystallization temperature (Tc
) as ENR content increases while the glass transition temperature (Tg
) remained unchanged.
Water absorption was observed to increase with ENR loadings. Increase in ENR content was also observed to reduce the
chemical resistance of the blends.
Feedstock preparation, as well as its characterization, is crucial in the production of highly sintered parts with minimal defect. The hard metal powder - particularly, cemented carbide (wc-co) used in this study was investigated both physically and thermally to determine its properties before the mixing and injection molding stage. Several analyses were conducted, such as scanning electron microscopy, energy dispersive X-ray diffraction, pycnometer density, critical powder volume percentage (cPvP), as well as thermal tests, such as thermogravimetric analysis and differential scanning calorimetry. On the basis of the CPVP value, the feedstock, consisting of wc-co powder, was mixed with 60% palm stearin and 40% polyethylene at an optimal powder loading, within 2 to 5% lower than the CPVP value. The CPVP spotted value was 65%. The feedstock optimal value at 61% showed good rheological properties (pseudoplastic behavior) with an n value lower than 1, considerably low activation energy and high moldability index. These preliminary properties of the feedstock serve as a benchmark in designing the schedule for the next whole steps (i.e. injection, debinding and sintering processes).
In this experimental study, a composite of poly-ether-ketone-ketone by reinforcement of hydroxyapatite and chitosan has been prepared for possible applications as orthopaedic scaffolds. Initially, different weight percentages of hydroxyapatite and chitosan were reinforced in the poly-ether-ketone-ketone matrix and tested for melt flow index in order to check the flowability of different compositions/proportions. Suitable compositions revealed by the melt flow index test were then taken forward for the extrusion of filament required for fused deposition modelling. For thermomechanical investigations, Taguchi-based design of experiments has been used with input variables in the extrusion process as follows: temperature, load applied and different composition/proportions. The specimens in the form of feedstock filament produced by the extrusion process were made to undergo tensile testing. The specimens were also inspected by differential scanning calorimetry and photomicrographs. Finally, the specimen showing the best performance from the thermomechanical viewpoint has been selected to extrude the filament for the fused deposition modelling process.