The enormous need of orthopaedic (surgical) implants such as osteosynthesis plates is difficult to be fulfilled in developing countries commonly rely on imported ones. One of the alternatives is utilization of local resources, but only after they have been proven safe to use, to overcome this problem. Surface properties are some of the determining factors of safety for those implants. We have succeeded in developing prototype of osteosynthesis plate and the results indicate that Indonesian-made plates need improvement with regards to the surface quality of physical characterization.
This work reports a new method to covalently attach calix[4]arene derivatives onto MCM-41, using a diisocyanate as a linker. The modified mesoporous silicates were characterized by fourier transform infrared spectroscopy (FTIR), thermal analysis (TGA) and elemental analysis. The FTIR spectra and TGA analysis verified that the calix[4]arene derivates are covalently attached to the mesoporous silica. The preservation of the MCM-41 channel system was checked by X-ray diffraction and nitrogen adsorption analysis.
Development of new materials for different applications especially as bio-composites has received great attention. This study concentrates on development of a biopolymer based on chitosan (CT) and halloysite nanotubes (HNT) and evaluates the copper removal intake as a potential application of this bio-composite. In this study, CT/HNT beads were prepared by ultrasonic-assisted extrusion-dripping method for the first time. Two sources of HNTs (i.e. Dragonite and Matauri Bay) were added into a chitosan solution (2wt.%) at various loading fractions (25, 50, 75wt.%). The effect of ultrasound as a mixing device was also studied by varying the amplitude at constant frequency of 25%, 50% and 75%. Characteristics and physical properties of the prepared CT/HNT beads were also analyzed by SEM, FTIR, TGA and BET the results show that introducing HNT to chitosan increases the adsorption capacity toward copper ions; however HNT loading fraction above 50wt.% resulted in a decrease in adsorption capacity attributed to limited accessibility of the amino groups. The adsorption capacity of the CT/HNT beads prepared from Dragonite source had a larger adsorption capacity of 14.2mg/g as compared to that of Matauri Bay, 10.55mg/g. It was observed that the adsorption capacity of the beads toward copper ions decreased when the loading fraction of HNT is increased at constant ultrasound amplitude. The result of this study helps to understand the links between the characteristics and adsorption abilities of CT/HNT beads.
In this study, hybrid montmorillonite/cellulose nanowhiskers (MMT/CNW) reinforced polylactic acid (PLA) nanocomposites were produced through solution casting. The CNW filler was first isolated from microcrystalline cellulose by chemical swelling technique. The partial replacement of MMT with CNW in order to produce PLA/MMT/CNW hybrid nanocomposites was performed at 5 parts per hundred parts of polymer (phr) fillers content, based on highest tensile strength values as reported in our previous study. MMT were partially replaced with various amounts of CNW (1, 2, 3, 4 and 5phr). The tensile, thermal, morphological and biodegradability properties of PLA hybrid nanocomposites were investigated. The highest tensile strength of hybrid nanocomposites was obtained with the combination of 4phr MMT and 1phr CNW. Interestingly, the ductility of hybrid nanocomposites increased significantly by 79% at this formulation. The Young's modulus increased linearly with increasing CNW content. Thermogravimetric analysis illustrated that the partial replacement of MMT with CNW filler enhanced the thermal stability of the PLA. This is due to the relatively good dispersion of fillers in the hybrid nanocomposites samples as revealed by transmission electron microscopy. Interestingly, partial replacements of MMT with CNW improved the biodegradability of hybrid nanocomposites compared to PLA/MMT and neat PLA.
This paper reports the post-processing ageing phenomena of thermoplastic sago starch (TPS) and plasticised sago pith waste (SPW), which were processed using twin-screw extrusion and compression moulding techniques. Wide angle X-ray diffraction (XRD) analyses showed that after processing, starch molecules rearranged into VH-type (which was formed rapidly right post processing and concluded within 4 days) and B-type (which was formed slowly over a period of months) crystallites. Evidence from Fourier transform infrared spectroscopy (FTIR) analyses corroborated the 2-stage crystallisation process, which observed changes in peak styles and peak intensities (at 1043 and 1026 cm-1) and bandnarrowing. Thermogravimetric analysis (TGA) studies showed that the thermal stability of plasticised SPW declined continuously for 90 days before gradual increments ensued. For all formulations tested, post-processing ageing led to drastic changes in the tensile strength (increased) and elongation at break (decreased). Glycerol and fibres restrained the retrogradation of starch molecules in TPS and SPW.
The aim of this study is to investigate natural cellulosic fibers extracted from Tridax procumbens plants. The obtained fibers were alkali treated for their effective usage as reinforcement in composites. The physical, chemical, crystallinity, thermal, wettability and surface characteristics were analyzed for raw, and alkali treated Tridax procumbens fibers (TPFs). The test results conclude that there was an increase in cellulose content with a reduction in hemicellulose, lignin, and wax upon alkali treatment. This enhanced the thermal stability, tensile strength, crystallinity, and surface roughness characteristics. The contact angle was also lesser for treated TPFs which prove its better wettability with the liquid phase. The Weibull distribution analysis was adopted for the analysis of the fiber diameter and tensile properties. Thus the considerable improvement in the properties of alkali treated TPFs would be worth for developing high-performance polymer composites.
Due to a huge increase in polymer production, a tremendous increase in municipal solid waste is observed. Every year the existing landfills for disposal of waste polymers decrease and the effective recycling techniques for waste polymers are getting more and more important. In this work pyrolysis of waste polystyrene was performed in the presence of a laboratory synthesized copper oxide. The samples were pyrolyzed at different heating rates that is, 5°Cmin-1, 10°Cmin-1, 15°Cmin-1 and 20°Cmin-1 in a thermogravimetric analyzer in inert atmosphere using nitrogen. Thermogravimetric data were interpreted using various model fitting (Coats-Redfern) and model free methods (Ozawa-Flynn-Wall, Kissinger-Akahira-Sunose and Friedman). Thermodynamic parameters for the reaction were also determined. The activation energy calculated applying Coats-Redfern, Ozawa-Flynn-Wall, Kissinger-Akahira-Sunose and Friedman models were found in the ranges 105-148.48 kJmol-1, 99.41-140.52 kJmol-1, 103.67-149.15 kJmol-1 and 99.93-141.25 kJmol-1, respectively. The lowest activation energy for polystyrene degradation in the presence of copper oxide indicates the suitability of catalyst for the decomposition reaction to take place at lower temperature. Moreover, the obtained kinetics and thermodynamic parameters would be very helpful in determining the reaction mechanism of the solid waste in a real system.
Liquid natural rubber (LNR) was functionalized into liquid epoxidized natural rubber (LENR) and hydroxylated LNR (LNROH)
via oxidation using a Na2
WO4
/CH3
COOH/H2
O2
catalytic system. Microstructures of LNR and functionalized LNRs
were characterized using Fourier Transform Infrared (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopies. The
effect of CH3
COOH, H2
O2
, Na2
WO4
, reaction time and temperature. reaction time and temperature on epoxy content were
investigated. LNR-OH was obtained when oxidation reaction was conducted at a longer reaction time, higher temperature
or excess amount of catalyst. Thermogravimetric analysis (TGA) reported the thermal behavior of functionalized LNRs.
Molecular weight and polydispersity index (PDI) were determined using gel permeation chromatography (GPC).
Chitosan-deep eutectic solvent (DES) beads were prepared from chitosan and DESs. The DESs used were choline chloride-urea (DES A) and choline chloride-glycerol (DES B). Both chitosan-DES beads were used to remove malachite green (MG) dye from an aqueous solution. The optimum pH for chitosan-DES A was recorded at pH 8.0 while optimum pH for chitosan-DES B was pH 9.0. The maximum adsorption capacity obtained for chitosan-DES A and chitosan-DES B were 6.54 mg/g and 8.64 mg/g, respectively. The optimum conditions for both chitosan-DES beads to remove MG were 0.08 g of adsorbent and 20 min of agitation time. Five kinetic models were applied to analyse the data and the results showed that the pseudo-second-order and intraparticle diffusion model fitted best with R2 > 0.999. For the adsorption capacity, results show that the Freundlich and Langmuir adsorption isotherms fitted well with chitosan-DES A and chitosan-DES B, respectively. The maximum adsorption capacities (qmax) obtained from chitosan-DES A and chitosan-DES B were 1.43 mg/g and 17.86 mg/g, respectively. Desorption indicated good performance in practical applications.
A study was carried out to determine the effectiveness of lignin, extracted from oil palm (Elaeis guineensis) biomass as water-in-oil (W/O) emulsifying agent. To achieve this goal, soda lignin (SL) was extracted via soda pulping process and a series of nanosized soda lignin (NSL) were prepared using homogenizer at three different speed i.e. 10,400 rpm (NSL 10), 11,400 rpm (NSL 11) and 12,400 rpm (NSL 12) for one hour. All prepared samples were characterized by FT-IR, UV-Vis spectroscopy, thermogravimetric analysis (TGA), zeta potential analyser, Transmission Electron Microscope (TEM) and Extreme High Resolution Field Emission Scanning Electron Microscope (XHR-FESEM). The result of FTIR showed that there is no prominent change occurred in spectra of all samples while a good stability was reflected by TGA curves. The percentage of creaming index and visual observations of all samples demonstrated that NSL 12 and dosage 2 g (out of 1 g, 1.5 g and 2 g) were found to be the best among all samples. Furthermore, the results of IFT indicate that NSL 12 was proven to be more stable than the commercial product. Therefore, NSL 12 is selected for toxicological studies and was found safe in both, in vitro and in vivo studies.
In current research work, chitosan (Chi) was subjected to subsequent physical and chemical modifications by incorporating kaolin clay (KA) into its polymeric structure, and crosslinking process with a covalent cross-linker namely epichlorohydrin (ECH) respectively. The final product of crosslinked chitosan-epichlorohydrin/kaolin (Chi-ECH/KA) composite was successfully applied for color removal and chemical oxygen demand (COD) reduction of textile dye namely reactive blue 19 dye (RB19) from aqueous environment. The influence of pertinent parameters, i.e. A: Chi-ECH/KA dose (0.02-0.1 g), B: pH (4-10), and C: time (5-30 min) on the RB19 color removal and COD reduction were statistically optimized by using response surface methodology with Box-Behnken design (RSM-BBD). The experimental data of the adsorption kinetic and the adsorption isotherm demonstrated a better fitness to pseudo-second order model and Langmuir isotherm model respectively. Excellent absorption ability of 560.9 mg/g was recorded for Chi-ECH/KA composite. The calculated thermodynamic functions clarified that the RB19 adsorption process was endothermic and spontaneous in nature. The mechanism of RB19 adsorption onto the Chi-ECH/KA may include electrostatic interactions, hydrogen bonding, Yoshida H-bonding, and n-π interactions. This study introduces Chi-ECH/KA composite as an eco-friendly, potential and multi-function composite bio adsorbent for removal of textile dye and COD reduction from aqueous environment.
To evaluate the possibilities for biofuel and bioenergy production Acacia Holosericea, which is an invasive plant available in Brunei Darussalam, was investigated. Proximate analysis of Acacia Holosericea shows that the moisture content, volatile matters, fixed carbon, and ash contents were 9.56%, 65.12%, 21.21%, and 3.91%, respectively. Ultimate analysis shows carbon, hydrogen, and nitrogen as 44.03%, 5.67%, and 0.25%, respectively. The thermogravimetric analysis (TGA) results have shown that maximum weight loss occurred for this biomass at 357 °C for pyrolysis and 287 °C for combustion conditions. Low moisture content (<10%), high hydrogen content, and higher heating value (about 18.13 MJ/kg) makes this species a potential biomass. The production of bio-char, bio-oil, and biogas from Acacia Holosericea was found 34.45%, 32.56%, 33.09% for 500 °C with a heating rate 5 °C/min and 25.81%, 37.61%, 36.58% with a heating rate 10 °C/min, respectively, in this research. From Fourier transform infrared (FTIR) spectroscopy it was shown that a strong C-H, C-O, and C=C bond exists in the bio-char of the sample.
In this study, we fabricated a modified biomaterial based on chitosan and gelatin, which is an intrinsic hydrophilic membrane for oil-water separation to clean water contamination by oil. Modification of the membrane with a non-toxic natural crosslinker, genipin, significantly enhanced the stability of the biopolymer membrane in a water-based medium towards an eco-friendly environment. The effects of various compositions of genipin-crosslinked chitosan-gelatin membrane on the rheological properties, thermal stability, and morphological structure of the membrane were investigated using a dynamic rotational rheometer, thermogravimetry analysis, and chemical composition by attenuated total reflectance spectroscopy (ATR). Modified chitosan-gelatin membrane showed completely miscible blends, as determined by field-emission scanning electron microscopy, differential scanning calorimetry, and ATR. Morphological results showed membrane with establish microstructure to further experiment as filtration product. The membranes were successfully tested for their oil-water separation efficiencies. The membrane proved to be selective and effective in separating water from an oil-water mixture. The optimum results achieved a stable microporous structure of the membrane (microfiltration) and a separation efficiency of above 98%. The membrane showed a high permeation flux, generated as high as 698 and 420 L m-2 h-1 for cooking and crude oils, respectively. Owing to its outstanding recyclability and anti-fouling performance, the membrane can be washed away easily, ensuring the reusability of the prepared membrane.
This dataset presents morphological features, elemental composition and functional groups of different pre- and post-gamma (γ)-irradiated chitosan (10kGy & 20kGy) prepared from shrimp waste. The γ-irradiated chitosan was characterized using Fourier transfer infrared (FTIR) spectroscopy and X-ray diffraction (XRD) analyses. Thermogravimetry/differential thermal analysis (TG/DTA) were performed using Perkin Elmer Pyris Diamond DSC with a heating rate of 10 °C/minute and dynamic synthetic atmospheric air set at flow rate of 100 ml/minute. We observed γ-irradiated chitosan to have shorter polymer size, small pores and compacted structure with active alkyl and hydroxyl groups when compared to non-irradiated chitosan. Our data provides baseline understanding for structure of shrimp chitosan after 60Co exposure which means, the biopolymer becomes more stable and is considered suitable for vast food industry applications.
Textile waste cellulose nanofibrillated fibre has been reported with excellent strength reinforcement ability in other biopolymers. In this research cellulose nanofibrilated fibre (CNF) was isolated from the textile waste cotton fabrics with combined supercritical carbon dioxide and high-pressure homogenisation. The isolated CNF was used to enhance the polylactic acid/chitin (PLA/chitin) properties. The properties enhancement effect of the CNF was studied by characterising the PLA/chitin/CNF biocomposite for improved mechanical, thermal, and morphological properties. The tensile properties, impact strength, dynamic mechanical analysis, thermogravimetry analysis, scanning electron microscopy, and the PLA/chitin/CNF biocomposite wettability were studied. The result showed that the tensile strength, elongation, tensile modulus, and impact strength improved significantly with chitin and CNF compared with the neat PLA. Furthermore, the scanning electron microscopy SEM (Scanning Electron Microscopy) morphological images showed uniform distribution and dispersion of the three polymers in each other, which corroborate the improvement in mechanical properties. The biocomposite's water absorption increased more than the neat PLA, and the contact angle was reduced. The results of the ternary blend compared with PLA/chitin binary blend showed significant enhancement with CNF. This showed that the three polymers' combination resulted in a better material property than the binary blend.
To overcome drawbacks in the conventional chemical route to synthesize eugenyl benzoate, immobilized Rhizomucor miehei lipase (RML) as the biocatalyst was proposed. The RML conjugated to a hybrid support consisting of biopolymers, chitosan (CS) and chitin nanowhiskers (CNWs). 1-ethyl-3-[3-dimethylaminopropyl]carbodiimide hydrochloride (EDAC) was used as the crosslinker to bind the lipase. Immobilization of RML was the highest on crosslinked CS/CNWs which gave a protein loading of ∼8.12 mg/g, corresponding to specific and residual activity of 537 U/g and 137%, respectively. Fourier transform infrared spectroscopy, thermogravimetric analysis-differential thermogravimetry, field emission scanning electron and atomic force microscopy of RML-CS/CNWs revealed that RML was successfully attached to the surface of crosslinked CS/CNWs. Under an optimized condition, the highest yield of eugenyl benzoate (56.3%) was attained after 5 h using 3 mg/mL of RML-CS/CNWs with molar ratio of eugenol: benzoic acid of 3:1, as compared to only 47.3% for the free RML. Analyses of FTIR and NMR on purified eugenyl benzoate affirmed that the ester was successfully produced in the enzymatic esterification. Therefore, the use of the RML-CS/CNWs biocatalysts appears promising to afford good yields of eugenyl benzoate within a relatively shorter reaction time.
Solid polymer electrolytes (SPEs) were prepared using rice starch as the polymer, sodium iodide (NaI) as the salt and 1-hexyl-3-methylimidazolium iodide (HMII) as the ionic liquid (IL). The solution casting technique was used for preparation of the PEs. The ionic conductivity and temperaturedependent properties of the PEs were measured and all the SPEs were found to follow the Arrhenius thermal activated model. Ionic conductivity increased as the percentage of ILs increased. The SPE containing 20% (wt) of HMII IL showed the highest ionic conductivity of 1.83×10-3 S/cm. Spectral and structural characterization of the PEs were performed by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD), respectively. The results of thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) indicate that the decomposition temperature (Tdc), glass transition temperatures (Tg) and melting points (Tm) shifted when complexation with HMII occurred. The PEs were used to fabricate dye-sensitized solar cells (DSSCs) and the DSSCs were analyzed under a 1-sun simulator. The SPE with the highest ionic conductivity displayed a short circuit current density (Jsc) of 9.07 (mA cm-2), open circuit voltage (Voc) of 0.58 (V), a fill factor (FF) of 0.65 and had the highest energy conversion efficiency of 3.42%.
Herein, hybrid k-carrageenan bio-nanocomposite films were fabricated by using two types of nanofillers, organically modified montmorillonite (OMMT), and cellulose nanocrystals (CNCs). Hybrid bio-nanocomposite films were made by casting techniques employing 4 wt% of CNCs, OMMT, and hybridized CNCs/OMMT in a 1:1 ratio. The rheological and morphological properties and thermal stability of all composites were investigated using rotational rheometry, thermogravimetry analysis, differential scanning calorimetry, field emission scanning electron microscopy, and transmission electron microscopy (TEM). The results showed that the hybrid CNC/OMMT bio-nanocomposite exhibited significantly improved properties as compared to those for the bio-nanocomposites with single fillers due to the nanosize and homogenous nanofiller dispersion in the matrix. Rheological analysis of the hybrid bio-nanocomposite showed higher dynamic shear storage modulus and complex viscosity values when compared to those for the bio-nanocomposite with individual fillers. The TEM analysis of the hybridized CNC/OMMT bio-nanocomposite revealed that more particles were packed together in the CNC network, which restricted the matrix mobility. The heat resistance and thermal stability bio-nanocomposite k-carrageenan film enhanced rapidly with the addition of hybridized CNCs/OMMT to 275 °C. The hybridized CNCs/OMMT exhibited synergistic effects due to the good affinity through interfacial interactions, resulting in the improvement of the material properties.
Liquefactions of kenaf core wood were carried out at different phenol-kenaf (P/k) ratios. Characterizations of kenaf core wood liquefied residue were carried out to measure the degree of liquefaction. This provides a new approach to understand some fundamental aspects of the liquefaction reaction. Functional groups on the raw kenaf core wood and liquefied residue were examined using Fourier transform infrared spectroscopy (FTIR). The crystallinity index of the kenaf wood liquefied residue, which represents crystallinity changes of the cellulose component after the liquefaction process, was studied using X-ray diffraction (XRD). The surface morphology of the wood residue was observed using scanning electron microscopy (SEM). The thermal behavior of the residues was analyzed using thermogravimetric analysis (TGA). Abroad peak around 3450-3400 cm-1 representing OH stretching in lignin start to disappear as P/K ratio increases. The results showed that the higher the P/K ratio the greater the liquefaction of the lignin component in the kenaf core wood. The crystallinity index (CrI) on the kenaf liquefied residues increased with the increase in P/K ratio. SEM images showed that the small fragments attached on the liquefied kenaf residue surface were gradually removed as the P/K ratio was increased from 1.5/1.0 to 2.5/1.0, which is mainly attributed to the greater chemical penetration toward reactive site of the kenaf fibres. Residue content decreased as the P/K ratio increased from 1.5/1.0 to 2.5/1.0. TGA results showed the increase of heat resistance in the residue as the P/K ratio was increased.
Determination of the thermal characteristics and temperature-dependent rheological properties of the magnetorheological elastomers (MREs) is of paramount importance particularly with regards to MRE applications. Hitherto, a paucity of temperature dependent analysis has been conducted by MRE researchers. In this study, an investigation on the thermal and rheological properties of epoxidized natural rubber (ENR)-based MREs was performed. Various percentages of carbonyl iron particles (CIPs) were blended with the ENR compound using a two roll-mill for the preparation of the ENR-based MRE samples. The morphological, elemental, and thermal analyses were performed before the rheological test. Several characterizations, as well as the effects of the strain amplitude, temperature, and magnetic field on the rheological properties of ENR-based MRE samples, were evaluated. The micrographs and elemental results were well-correlated regarding the CIP and Fe contents, and a uniform distribution of CIPs was achieved. The results of the thermal test indicated that the incorporation of CIPs enhanced the thermal stability of the ENR-based MREs. Based on the rheological analysis, the storage modulus and loss factor were dependent on the CIP content and strain amplitude. The effect of temperature on the rheological properties revealed that the stiffness of the ENR-based MREs was considered stable, and they were appropriate to be employed in the MRE devices exposed to high temperatures above 45 °C.