The aim was to explore the utilization of tea leaf waste fibers (TLWF) as a source for the production of cellulose nanocrystals (CNC). TLWF was first treated with alkaline, followed by bleaching before being hydrolyzed with concentrated sulfuric acid. The materials attained after each step of chemical treatments were characterized and their chemical compositions were studied. The structure analysis was examined by Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). From FTIR analysis, two peaks at 1716 and 1207 cm-1-which represent C=O stretching and C⁻O stretching, respectively-disappeared in the spectra after the alkaline and bleaching treatments indicated that hemicellulose and lignin were almost entirely discarded from the fiber. The surface morphology of TLWF before and after chemical treatments was investigated by scanning electron microscopy (SEM) while the dimension of CNC was determined by transmission electron microscopy (TEM). The extraction of CNC increased the surface roughness and the crystallinity index of fiber from 41.5% to 83.1%. Morphological characterization from TEM revealed the appearance of needle-like shaped CNCs with average diameter of 7.97 nm. The promising results from all the analyses justify TLWF as a principal source of natural materials which can produce CNC.
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.
Surface modified Multi-walled carbon nanotubes (MWCNTs) Buckypaper/Polyvinyl Alcohol (BP/PVA) composite membrane was synthesized and utilized as support material for immobilization of Jicama peroxidase (JP). JP was successfully immobilized on the BP/PVA membrane via covalent bonding by using glutaraldehyde. The immobilization efficiency was optimized using response surface methodology (RSM) with the face-centered central composite design (FCCCD) model. The optimum enzyme immobilization efficiency was achieved at pH 6, with initial enzyme loading of 0.13 U/mL and immobilization time of 130 min. The results of BP/PVA membrane showed excellent performance in immobilization of JP with high enzyme loading of 217 mg/g and immobilization efficiency of 81.74%. The immobilized system exhibited significantly improved operational stability under various parameters, such as pH, temperature, thermal and storage stabilities when compared with free enzyme. The effective binding of peroxidase on the surface of the BP/PVA membrane was evaluated and confirmed by Field emission scanning electron microscopy (FESEM) coupled with Energy Dispersive X-Ray Spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR) and Thermogravimetric Analysis (TGA). This work reports the characterization results and performances of the surface modified BP/PVA membrane for peroxidase immobilization. The superior properties of JP-immobilized BP/PVA membrane make it promising new-generation nanomaterials for industrial applications.
The aim of this study was ultrasound assisted removal of Ceftriaxone sodium (CS) based on CCD model. Using sonochemical synthesized Bi2WO6 implanted on graphitic carbon nitride/Multiwall carbon nanotube (g-C3N4/MWCNT/Bi2WO6). For this purpose g-C3N4/MWCNT/Bi2WO6 was synthesized and characterized using diverse approaches including XRD, FE-SEM, XPS, EDS, HRTEM, FT-IR. Then, the contribution of conventional variables including pH, CS concentration, adsorbent dosage and ultrasound contact time were studied by central composite design (CCD) under response surface methodology (RSM). ANOVA was employed to the variable factors, and the most desirable operational conditions mass provided. Drug adsorption yield of 98.85% obtained under these defined conditions. Through conducting five experiments, the proper prediction of the optimum point were examined. The respective results showed that RSD% was lower than 5% while the t-test confirmed the high quality of fitting. Langmuir isotherm equation fits the experimental data best and the removal followed pseudo-second order kinetics. The estimation of the experimentally obtained maximum adsorption capacities was 19.57 mg.g- of g-C3N4/MWCNT/Bi2WO6 for CS. Boundary layer diffusion explained the mechanism of removal via intraparticle diffusion.
Natural fiber composites have been widely used for various applications such as automotive components, aircraft components and sports equipment. Among the natural fibers Typha spp have gained considerable attention to replace synthetic fibers due to their unique nature. The untreated and alkali-treated fibers treated in different durations were dried under the sun for 4 h prior to the fabrication of Typha fiber reinforced epoxy composites. The chemical structure and crystallinity index of composites were examined via FT-IR and XRD respectively. The tensile, flexural and impact tests were conducted to investigate the effect of the alkali treated Typha fibers on the epoxy composite. From the microscopy analysis, it was observed that the fracture mechanism of the composite was due to the fiber and matrix debonding, fiber pull out from the matrix, and fiber damage. The tensile, flexural and impact strength of the Typha fiber reinforced epoxy composite were increased after 5% alkaline immersion compared to untreated Typha fiber composite. From these results, it can be concluded that the alkali treatment on Typha fiber could improve the interfacial compatibility between epoxy resin and Typha fiber, which resulted in the better mechanical properties and made the composite more hydrophobic. So far there is no comprehensive report about Typha fiber reinforcing epoxy composite, investigating the effect of the alkali treatment duration on the interfacial compatibility, and their effect on chemical and mechanical of Typha fiber reinforced composite, which plays a vital role to provide the overall mechanical performance to the composite.
A halloysite nanotubes⁻polyvinyl alcohol⁻polyvinylpyrrolidone (HNTs⁻PVA⁻PVP) composite has been investigated for a quite long time aiming at improving the physico⁻chemical characterization of HNTs. In this work, HNTs⁻PVA⁻PVP composite were prepared based on a unique procedure characterized by crosslinking two polymers with HNTs. The composite of two polymers were modified by treating HNTs with phosphoric acid (H₃PO₄) and by using malonic acid (MA) as a crosslinker. The composite was also treated by adding the dispersion agent sodium dodecyl sulfate (SDS). The HNTs⁻PVA⁻PVP composite shows better characteristics regarding agglomeration when HNTs is treated in advance by H₃PO₄. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), brunauer⁻emmett⁻teller (BET), size distribution, and atomic force microscopy (AFM) are used to characterize the physio-chemical properties of the composite. FTIR shows additional peaks at 2924.29, 1455.7, and 682.4 cm-1 compared to the neat HNTs due to adding MA. Despite that, the XRD spectra do not show a significant difference, the decrease in peak intensity could be attributed to the addition of semi-crystalline PVA and the amorphous PVP. The images taken by TEM and FESEM show the possible effects of MA on the morphology and internal feature of HNTs⁻PVA⁻PVP composite treated by MA by showing the deformation of the matrix. The BET surface area increased to 121.1 m²/g compared to the neat HNTs at 59.1 m²/g. This result, the second highest recorded result, is considered a breakthrough in enhancing the properties of HNTs⁻PVA⁻PVP composite, and treatment by MA crosslinking may attribute to the size and the number of the pores. The results from these techniques clearly showed that a significant change has occurred for treated HNTs⁻PVA⁻PVP composite where MA was added. The characterization of HNTs⁻PVA⁻PVP composite with and without treating HNTs and using crosslinker may lead to a better understanding of this new composites as a precursor to possible applications in the dentistry field.
The objective of this work is to characterize and investigate the blood compatibility of polyurethane (PU)/mustard oil composites fabricated using electrospinning technique. The fabricated scaffold was characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), thermogravimetric analysis (TGA) and contact angle measurements. The activated partial thromboplastin time (APPT), prothrombin time (PT) and the hemolytic assay were done to investigate the blood compatibility of the developed composites. The SEM results revealed that the fiber diameter of the composites (761 ± 123 nm) was reduced compared to pristine PU control. The interaction between PU and mustard oil was confirmed by FTIR as evident through the shifting of peaks. The fabricated composites depicted hydrophobic behavior as insinuated by the increase in contact angle measurements. PU/mustard composites displayed improved crystallinity as confirmed by TGA. Atomic force micrographs suggested that developed PU/mustard oil composites showed an increase in the surface roughness (Ra) compared to pure PU. The Ra of pure PU was observed to be 723 nm but for the fabricated PU/mustard oil composite the Ra was found to be 1298 nm (Ra). The hemolytic index value for pure PU and fabricated composites was observed to be 2.73% and 1.15% indicating that developed composites showed a non-hemolytic behavior signifying the safety of the composites with red blood cells. Hence the newly developed composites with improved physicochemical and blood compatibility properties may be considered as a potential candidate for fabricating cardiac patches and grafts.
Gamma-ray radiation was used as a clean and easy method for turning the physicochemical properties of graphene oxide (GO) in this study. Silane functionalized-GO were synthesized by chemically grafting 3-aminopropyltriethoxysilane (APTES) and 3-glycidyloxypropyltrimethoxysilane (GPTES) onto GO surface using gamma-ray irradiation. This established non-contact process is used to create a reductive medium which is deemed simpler, purer and less harmful compared conventional chemical reduction. The resulting functionalized-GO were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), and Raman spectroscopy. The chemical interaction of silane with the GO surface was confirmed by FT-IR. X-ray diffraction reveals the change in the crystalline phases was due to surface functionalization. Surface defects of the GO due to the introduction of silane mioties was revealed by Raman spectroscopy. Thermogravimetric analysis of the functionalized-GO exhibits a multiple peaks in the temperature range of 200-650 °C which corresponds to the degradation of chemically grafted silane on the GO surface.
The aim was to explore the utilization of oil palm mesocarp fiber (OPMF) as a source for the production of cellulose nanocrystals (CNC). OPMF was first treated with alkali and then bleached before the production of CNC by acid hydrolysis (H₂SO₄). The produced materials were characterized using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), a scanning electron microscope (SEM) and a transmission electron microscope (TEM). It was proven that acid hydrolysis can increase the crystallinity of bleached OPMF and reduce the dimension of cellulose to nano scale. Changes in the peaks of the FTIR spectrum at 2852 (C-H stretching), 1732 (C=O stretching) and 1234 cm-1 (C-O stretching) indicated that the alkali treatment completely removed hemicelluloses and lignin from the fiber surface. This can be seen from the thermogram obtained from the TGA characterization. Morphological characterization clearly showed the formation of rod-shaped CNCs. The promising results prove that OPMF is a valuable source for the production of CNC.
Pectin is an anionic, water-soluble polymer predominantly consisting of covalently 1,4-linked α-d-galacturonic acid units. This naturally occurring, renewable and biodegradable polymer is underutilized in polymer science due to its insolubility in organic solvents, which renders conventional polymerization methods impractical. To circumvent this problem, cerium-initiated radical polymerization was utilized to graft methoxy-poly(ethylene glycol) methacrylate (mPEGMA) onto pectin in water. The copolymers were characterized by ¹H nuclear magnetic resonance (NMR), Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA), and used in the formation of supramolecular hydrogels through the addition of α-cyclodextrin (α-CD) to induce crosslinking. These hydrogels possessed thixotropic properties; shear-thinning to liquid upon agitation but settling into gels at rest. In contrast to most of the other hydrogels produced through the use of poly(ethylene glycol) (PEG)-grafted polymers, the pectin-PEGMA/α-CD hydrogels were unaffected by temperature changes.
Nanocomposite polymer electrolyte membranes (NCPEMs) based on poly(acrylic acid)(PAA) and titania (TiO₂) are prepared by a solution casting technique. The ionic conductivity of NCPEMs increases with the weight ratio of TiO₂.The highest ionic conductivity of (8.36 ± 0.01) × 10-4 S·cm-1 is obtained with addition of 6 wt % of TiO₂ at ambient temperature. The complexation between PAA, LiTFSI and TiO₂ is discussed in Attenuated total reflectance-Fourier Transform Infrared (ATR-FTIR) studies. Electrical double layer capacitors (EDLCs) are fabricated using the filler-free polymer electrolyte or the most conducting NCPEM and carbon-based electrodes. The electrochemical performances of fabricated EDLCs are studied through cyclic voltammetry (CV) and galvanostatic charge-discharge studies. EDLC comprising NCPEM shows the specific capacitance of 28.56 F·g-1 (or equivalent to 29.54 mF·cm-2) with excellent electrochemical stability.
Cadmium oxide semiconductor nanoparticles were produced using a water based mixture, incorporating cadmium nitrates, polyvinyl pyrrolidone (PVP), and calcination temperature. An X-ray diffraction (XRD) evaluation was conducted to determine the degree of crystallization of the semiconductor nanoparticles. In addition, scanning electron microscopy (SEM) was conducted to identify the morphological features of the nanoparticles. The typical particle sizes and particle dispersal were analyzed via the use of transmission electron microscopy (TEM). The findings provided further support for the XRD outcomes. To determine the composition phase, Fourier transform infrared spectroscopy (FT-IR) was conducted, as it indicated the existence of not only metal oxide ionic band in the selection of samples, but also the efficient removal of organic compounds following calcinations. The optical characteristics were demonstrated, so as to analyze the energy band gap via the use of a UV⁻Vis spectrophotometer. A reduced particle size resulted in diminution of the intensity of photoluminescence, was demonstrated by PL spectra. Plus, the magnetic characteristics were examined using an electron spin resonance (ESR) spectroscopy, which affirmed the existence of unpaired electrons.
One of the approaches to prolong the service lifespan of polymeric material is the development of self-healing ability by means of embedded microcapsules containing a healing agent. In this work, poly(melamine-urea-formaldehyde) (PMUF) microcapsules containing a palm oil-based alkyd were produced by polymerization of melamine resin, urea and formaldehyde that encapsulated droplets of the suspended alkyd particles. A series of spherical and free-flowing microcapsules were obtained. The chemical properties of core and shell materials were characterized by Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) and proton nuclear magnetic resonance spectroscopy (¹H-NMR). Differential scanning calorimetry (DSC) analysis showed a glass transition around -15 °C due to the alkyd, and a melting temperature at around 200 °C due to the shell. Thermogravimetric analysis (TGA) results showed that the core and shell thermally degraded within the temperature range of 200⁻600 °C. Field emission scanning electron microscope (FESEM) examination of the ruptured microcapsule showed smooth inner and rough outer surfaces of the shell. Flexural strength and microhardness (Vickers) of the cured epoxy compound were not affected with the incorporation of 1%⁻3% of the microcapsules. The viability of the healing reactions was demonstrated by blending small amounts of alkyd with epoxy and hardener at different ratios. The blends could readily cure to non-sticky hard solids at room temperature and the reactions could be verified by ATR-FTIR.
In this paper, novel zwitterionic graphene oxide (GO) nanohybrid was synthesized using monomers [2-(Methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide (SBMA) and N,N'-methylenebis(acrylamide) (MBAAm) (GO@poly(SBMA-co-MBAAm), and incorporated into polysulfone (PSF) hollow fiber membrane for the effectual rejection of dye from the wastewater. The synthesized nanohybrid was characterized using FT-IR, PXRD, TGA, EDX, TEM and zeta potential analysis. The occurrence of nanohybrid on the membrane matrix and the elemental composition were analyzed by XPS. The as-prepared tight ultrafiltration hollow fiber membrane exhibited high rejection of reactive black 5 (RB-5, 99%) and reactive orange 16 (RO-16, 74%) at a dye concentration of 10 ppm and pure water flux (PWF) of 49.6 L/m2h. Fabricated nanocomposite membranes were also studied for their efficacy in the removal of both monovalent (NaCl) and divalent salts (Na2SO4). The results revealed that the membrane possesses complete permeation to NaCl with less rejection of Na2SO4 (<5%). In addition, the nanocomposite membrane revealed outstanding antifouling performance with the flux recovery ratio (FRR) of 73% towards bovine serum albumin (BSA). Therefore, the in-house prepared novel nanocomposite membrane is a good candidate for the effective decolorization of wastewater containing dye.
Diosgenin encapsulated PCL-Pluronic nanoparticles (PCL-F68-D-NPs) were developed using the nanoprecipitation method to improve performance in brain cancer (glioblastoma) therapy. The nanoparticles were characterized by dynamic light scattering (DLS)/Zeta potential, Fourier-transform infrared (FTIR) spectra, X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), and Transmission electron microscopy (TEM). The encapsulation efficiency, loading efficiency, and yield were calculated. The in vitro release rate was determined, and the kinetic model of diosgenin release was plotted and ascertained. The cytotoxicity was checked by MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide)assay against U87-MG cells (glioblastoma cell lines). The obtained nanoparticles demonstrated good size distribution, stability, morphology, chemical, and mechanical properties. The nanoparticles also possessed high encapsulation efficiency, loading efficiency, and yield. The release rate of Diosgenin was shown in a sustained manner. The in vitro cytotoxicity of PCL-F68-D-NPs showed higher toxicity against U87-MG cells than free Diosgenin.
In this work, a pair of biopolymer materials has been used to prepare high ion-conducting electrolytes for energy storage application (ESA). The chitosan:methylcellulose (CS:MC) blend was selected as a host for the ammonium thiocyanate NH4SCN dopant salt. Three different concentrations of glycerol was successfully incorporated as a plasticizer into the CS-MC-NH4SCN electrolyte system. The structural, electrical, and ion transport properties were investigated. The highest conductivity of 2.29 × 10-4 S cm-1 is recorded for the electrolyte incorporated 42 wt.% of plasticizer. The complexation and interaction of polymer electrolyte components are studied using the FTIR spectra. The deconvolution (DVN) of FTIR peaks as a sensitive method was used to calculate ion transport parameters. The percentage of free ions is found to influence the transport parameters of number density (n), ionic mobility (µ), and diffusion coefficient (D). All electrolytes in this work obey the non-Debye behavior. The highest conductivity electrolyte exhibits the dominancy of ions, where the ionic transference number, tion value of (0.976) is near to infinity with a voltage of breakdown of 2.11 V. The fabricated electrochemical double-layer capacitor (EDLC) achieves the highest specific capacitance, Cs of 98.08 F/g at 10 mV/s by using the cyclic voltammetry (CV) technique.
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.
Biobased polymers are useful materials in substituting conventional petroleum-derived polymers because of their good properties, ready availability, and abundance in nature. This study reports a new jatropha oil-based gel polymer electrolyte (GPE) for use in dye-sensitized solar cells (DSSCs). The GPE was prepared by mixing jatropha oil-based polyurethane acrylate (PUA) with different concentrations of lithium iodide (LiI). The GPE was characterized by infrared spectroscopy, thermal analysis, lithium nuclear magnetic resonance analysis, electrochemical analysis, and photocurrent conversion efficiency. The highest room-temperature ionic conductivity of 1.88 × 10-4 S cm-1 was obtained at 20 wt % of LiI salt. Additionally, the temperature-dependent ionic conductivity of the GPE exhibited Arrhenius behavior with an activation energy of 0.42 eV and a pre-exponential factor of 1.56 × 103 S cm-1. The electrochemical stability study showed that the PUA GPE was stable up to 2.35 V. The thermal stability of the gel electrolyte showed an improvement after the addition of the salt, suggesting a strong intermolecular interaction between PUA and Li, which leads to polymer-salt complexation, as proven by Fourier transform infrared spectroscopy analysis. A DSSC has been assembled using the optimum ionic conductivity gel electrolyte which indicated 1.2% efficiency under 1 sun condition. Thus, the jatropha oil-based GPE demonstrated favorable properties that make it a promising alternative to petroleum-derived polymer electrolytes in DSSCs.
In this study, solid polymer blend electrolytes (SPBEs) based on chitosan (CS) and methylcellulose (MC) incorporated with different concentrations of ammonium fluoride (NH4F) salt were synthesized using a solution cast technique. Both Fourier transformation infrared spectroscopy (FTIR) and X-ray diffraction (XRD) results confirmed a strong interaction and dispersion of the amorphous region within the CS:MC system in the presence of NH4F. To gain better insights into the electrical properties of the samples, the results of electrochemical impedance spectroscopy (EIS) were analyzed by electrical equivalent circuit (EEC) modeling. The highest conductivity of 2.96 × 10-3 S cm-1 was recorded for the sample incorporated with 40 wt.% of NH4F. Through transference number measurement (TNM) analysis, the fraction of ions was specified. The electrochemical stability of the electrolyte sample was found to be up to 2.3 V via the linear sweep voltammetry (LSV) study. The value of specific capacitance was determined to be around 58.3 F/g. The stability test showed that the electrical double layer capacitor (EDLC) system can be recharged and discharged for up to 100 cycles with an average specific capacitance of 64.1 F/g. The synthesized EDLC cell was found to exhibit high efficiency (90%). In the 1st cycle, the values of internal resistance, energy density and power density of the EDLC cell were determined to be 65 Ω, 9.3 Wh/kg and 1282 W/kg, respectively.
Being biodegradable and biocompatible are crucial characteristics for biomaterial used for medical and biomedical applications. Vegetable oil-based polyols are known to contribute both the biodegradability and biocompatibility of polyurethanes; however, petrochemical-based polyols were often incorporated to improve the thermal and mechanical properties of polyurethane. In this work, palm oil-based polyester polyol (PPP) derived from epoxidized palm olein and glutaric acid was reacted with isophorone diisocyanate to produce an aliphatic polyurethane, without the incorporation of any commercial petrochemical-based polyol. The effects of water content and isocyanate index were investigated. The polyurethanes produced consisted of > 90% porosity with interconnected micropores and macropores (37-1700 µm) and PU 1.0 possessed tensile strength and compression stress of 111 kPa and 64 kPa. The polyurethanes with comparable thermal stability, yet susceptible to enzymatic degradation with 7-59% of mass loss after 4 weeks of treatment. The polyurethanes demonstrated superior water uptake (up to 450%) and did not induce significant changes in pH of the medium. The chemical changes of the polyurethanes after enzymatic degradation were evaluated by FTIR and TGA analyses. The polyurethanes showed cell viability of 53.43% and 80.37% after 1 and 10 day(s) of cytotoxicity test; and cell adhesion and proliferation in cell adhesion test. The polyurethanes produced demonstrated its potential as biomaterial for soft tissue engineering applications.