This study was aimed at fabricating composites of polylactic acid (PLA) matrix-reinforced oil palm empty fruit bunch (OPEFB) fiber filled with chemically reduced graphene oxide (rGO). A total of 2-8 wt.% rGO/OPEFB/PLA composites were characterized for their complex permittivity using an open-ended coaxial probe (OEC) technique. The shielding efficiency properties were calculated using the measured transmission (S21) and the reflection (S11) coefficient results. All the measurements and calculations were performed in the 8-12 GHz frequency range. The morphological and microstructural study included X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and Fourier transform infrared spectroscopy (FTIR). The results indicated that the incorporation of rGO as filler into the composites enhanced their complex permittivity properties. The composites showed a total shielding efficiency (SET) of about 31.2 dB at a frequency range of 8-12 GHz, which suggests their usefulness for microwave absorption.
Various types of activated carbon nanofibers' (ACNFs) composites have been extensively studied and reported recently due to their extraordinary properties and applications. This study reports the fabrication and assessments of ACNFs incorporated with graphene-based materials, known as gACNFs, via simple electrospinning and subsequent physical activation process. TGA analysis proved graphene-derived rice husk ashes (GRHA)/ACNFs possess twice the carbon yield and thermally stable properties compared to other samples. Raman spectra, XRD, and FTIR analyses explained the chemical structures in all resultant gACNFs samples. The SEM and EDX results revealed the average fiber diameters of the gACNFs, ranging from 250 to 400 nm, and the successful incorporation of both GRHA and reduced graphene oxide (rGO) into the ACNFs' structures. The results revealed that ACNFs incorporated with GRHA possesses the highest specific surface area (SSA), of 384 m2/g, with high micropore volume, of 0.1580 cm3/g, which is up to 88% of the total pore volume. The GRHA/ACNF was found to be a better adsorbent for CH4 compared to pristine ACNFs and reduced graphene oxide (rGO/ACNF) as it showed sorption up to 66.40 mmol/g at 25 °C and 12 bar. The sorption capacity of the GRHA/ACNF was impressively higher than earlier reported studies on ACNFs and ACNF composites. Interestingly, the CH4 adsorption of all ACNF samples obeyed the pseudo-second-order kinetic model at low pressure (4 bar), indicating the chemisorption behaviors. However, it obeyed the pseudo-first order at higher pressures (8 and 12 bar), indicating the physisorption behaviors. These results correspond to the textural properties that describe that the high adsorption capacity of CH4 at high pressure is mainly dependent upon the specific surface area (SSA), pore size distribution, and the suitable range of pore size.
In this study, an optimized mesoporous sulfonated carbon (OMSC) catalyst derived from palm kernel shell biomass was developed using template carbonization and subsequent sulfonation under different temperatures and time conditions. The OMSC catalyst was characterized using acid-base titration, elemental analysis, XRD, Raman, FTIR, XPS, TPD-NH3, TGA-DTA, SEM, and N2 adsorption-desorption analysis to reveal its properties. Results proved that the OMSC catalyst is mesoporous and amorphous in structure with improved textural, acidic, and thermal properties. Both FTIR and XPS confirmed the presence of -SO3H, -OH, and -COOH functional groups on the surface of the catalyst. The OMSC catalyst was found to be efficient in catalyzing glycerol conversion to acetin via an acetylation reaction with acetic acid within a short period of 3 h. Response surface methodology (RSM), based on a two-level, three-factor, face-centered central composite design, was used to optimize the reaction conditions. The results showed that the optimized temperature, glycerol-to-acetic acid mole ratio, and catalyst load were 126 °C, 1:10.4, and 0.45 g, respectively. Under these optimum conditions, 97% glycerol conversion (GC) and selectivities of 4.9, 27.8, and 66.5% monoacetin (MA), diacetin (DA), and triacetin (TA), respectively, were achieved and found to be close to the predicted values. Statistical analysis showed that the regression model, as well as the model terms, were significant with the predicted R2 in reasonable agreement with the adjusted R2 (<0.2). The OMSC catalyst maintained excellent performance in GC for the five reaction cycles. The selectivity to TA, the most valuable product, was not stable until the fourth cycle, attributable to the leaching of the acid sites.
Nitrogen doped titanium dioxide (N-doped TiO2
) was synthesized by microwave using urea as nitrogen sources with
commercially available TiO2
-P25. The N-doped TiO2
was compared with unmodified TiO2
by carrying out the investigation
on its properties using x-ray diffraction (XRD) analysis, Brunauer-Emmett-Teller (BET), Fourier transformed infrared
spectroscopy (FTIR) and diffuse reflectance spectroscopy (UV-Vis DRS). The photocatalytic activities of N-doped TiO2
and unmodified TiO2 were studied for photodegradation of reactive red 4 (RR4) under light emitting diode (LED) light
irradiation. An active photoresponse under LED light irradiation was observed from N-doped TiO2
with 60 min of time
irradiation to complete RR4 color removal while no photocatalytic degradation was observed from unmodified.
This present research aims to synthesize and investigate the adsorption potential of sugarcane bagasse (SCB) impregnated with iron oxide (Fe3O4) for dye removal. The surface morphology and functional groups of the newly developed adsorbent (ISCB) were studied using Scanning Electron Microscopy/Energy-dispersive X-ray spectroscopy (SEM/EDX), Fourier transforms infrared spectroscopy (FTIR), and X-ray powder diffraction (XRD) analysis. The effects of the operating parameters, including initial dye concentration, adsorbent dosage, contact time and initial pH of the dye solution on the adsorption efficiency were investigated to identify an optimal condition. The characterization of SEM-EDX and FTIR analyses shows that ISCB has a porous structure and carbon-containing functional groups. The adsorption result revealed that ISCB removed 93.7% of dye, 88.8% of color and had a dye adsorption capacity of 7.2 mg/g within 6 h of contact time using 0.7 g/L of ISCB at pH 8.4. The result obtained fitted well for Langmuir isotherms, and adsorption process followed the pseudo-second-order kinetic model. In conclusion, this study proved that ISCB has the potential to be used as an effective and low-cost adsorbent to remove dyes from wastewater.
Currently, the authentication of virgin coconut oil (VCO) has become very important due to the possible adulteration of VCO with cheaper plant oils such as corn (CO) and sunflower (SFO) oils. Methods involving Fourier transform mid infrared (FT-MIR) spectroscopy combined with chemometrics techniques (partial least square (PLS) and discriminant analysis (DA)) were developed for quantification and classification of CO and SFO in VCO. MIR spectra of oil samples were recorded at frequency regions of 4000-650cm-1 on horizontal attenuated total reflectance (HATR) attachment of FTIR. DA can successfully classify VCO and that adulterated with CO and SFO using 10 principal components. Furthermore, PLS model correlates the actual and FTIR estimated values of oil adulterants (CO and SFO) with coefficient of determination (R2) of 0.999.
Nanosilica particles were utilized as secondary reinforcement to enhance the strength of the epoxy resin matrix. Thin glass fibre reinforced polymer (GFRP) composite laminates of 3 ± 0.25 mm were developed with E-Glass mats of 610 GSM and LY556 epoxy resin. Nanosilica fillers were mixed with epoxy resin in the order of 0.25, 0.5, 0.75 and 1 wt% through mechanical stirring followed by an ultrasonication method. Thereafter, the damage was induced on toughened laminates through low-velocity drop weight impact tests and the induced damage was assessed through an image analysis tool. The residual compression strength of the impacted laminates was assessed through compression after impact (CAI) experiments. Laminates with nanosilica as secondary reinforcement exhibited enhanced compression strength, stiffness, and damage suppression. Results of Fourier-transform infrared spectroscopy revealed that physical toughening mechanisms enhanced the strength of the nanoparticle-reinforced composite. Failure analysis of the damaged area through scanning electron microscopy (SEM) evidenced the presence of key toughening mechanisms like damage containment through micro-cracks, enhanced fiber-matrix bonding, and load transfer.
We demonstrate the preparation of nanostructures cobalt oxide/reduced graphene oxide (Co3O4/rGO) nanocomposites by a simple one-step cost-effective hydrothermal technique for possible electrode materials in supercapacitor application. The X-ray diffraction patterns were employed to confirm the nanocomposite crystal system of Co3O4/rGO by demonstrating the existence of normal cubic spinel structure of Co3O4 in the matrix of Co3O4/rGO nanocomposite. FTIR and FT-Raman studies manifested the structural behaviour and quality of prepared Co3O4/rGO nanocomposite. The optical properties of the nanocomposite Co3O4/rGO have been investigated by UV absorption spectra. The SEM/TEM images showed that the Co3O4 nanoparticles in the Co3O4/rGO nanocomposites were covered over the surface of the rGO sheets. The electrical properties were analyzed in terms of real and imaginary permittivity, dielectric loss and AC conductivity. The electrocatalytic activities of synthesized Co3O4/rGO nanocomposites were determined by cyclic voltammetry and charge-discharge cycle to evaluate the supercapacitive performance. The specific capacitance of 754 Fg-1 was recorded for Co3O4/rGO nanocomposite based electrode in three electrode cell system. The electrode material exhibited an acceptable capability and excellent long-term cyclic stability by maintaining 96% after 1000 continuous cycles. These results showed that the prepared sample could be an ideal candidate for high-energy application as electrode materials. The synthesized Co3O4/rGO nanocomposite is a versatile material and can be used in various application such as fuel cells, electrochemical sensors, gas sensors, solar cells, and photocatalysis.
The exploitation of epoxidized natural rubber (ENR) in electrochemical applications is approaching its limits because of its poor thermo-mechanical properties. These properties could be improved by chemical and/or physical modification, including grafting and/or crosslinking techniques. In this work, acrylonitrile (ACN) has been successfully grafted onto ENR- 25 by a radical photopolymerization technique. The effect of (ACN to ENR) mole ratios on chemical structure and interaction, thermo-mechanical behaviour and that related to the viscoelastic properties of the polymer was investigated. The existence of the -C≡N functional group at the end-product of ACN-g-ENR is confirmed by infrared (FT-IR) and nuclear magnetic resonance (NMR) analyses. An enhanced grafting efficiency (~57%) was obtained after ACN was grafted onto the isoprene unit of ENR- 25 and showing a significant improvement in thermal stability and dielectric properties. The viscoelastic behaviour of the sample analysis showed an increase of storage modulus up to 150 × 103 MPa and the temperature of glass transition (Tg) was between -40 and 10 °C. The loss modulus, relaxation process, and tan delta were also described. Overall, the ACN-g-ENR shows a distinctive improvement in characteristics compared to ENR and can be widely used in many applications where natural rubber is used but improved thermal and mechanical properties are required. Likewise, it may also be used in electronic applications, for example, as a polymer electrolyte in batteries or supercapacitor.
Carbonized natural filler can offer the production of low cost composites with an eco-friendliness value. The evolving field of electronics encourages the exploration of more functions and potential for carbonized natural filler, such as by modifying its surface chemistry. In this work, we have performed surface modification on carbonized wood fiber (CWF) prior to it being used as filler in the ethylene vinyl acetate (EVA) composite system. Zinc chloride (ZnCl2) with various contents (2 to 8 wt%) was used to surface modify the CWF and the effects of ZnCl2 composition on the surface morphology and chemistry of the CWF filler were investigated. Furthermore, the absorptive, mechanical, thermal, and electrical properties of the EVA composites containing CWF-ZnCl2 were also analyzed. SEM images indicated changes in the morphology of the CWF while FTIR analysis proved the presence of ZnCl2 functional groups in the CWF. EVA composites incorporating the CWF-ZnCl2 showed superior mechanical, thermal and electrical properties compared to the ones containing the CWF. The optimum content of ZnCl2 was found to be 6 wt%. Surface modification raised the electrical conductivity of the EVA/CWF composite through the development of conductive deposits in the porous structure of the CWF as a channel for ionic and electronic transfer between the CWF and EVA matrix.
The potential of new trimetallic (Ce, Cu, La) loaded montmorillonite clay catalyst for synthesizing biodiesel using novel non-edible Celastrus paniculatus Willd seed oil via two-step transesterification reaction has been reported along with catalyst characterization. Transesterification reaction was optimized and maximum biodiesel yield of 89.42% achieved under optimal operating reaction states like; 1:12 oil to methanol ratio, 3.5% of catalyst amount, 120 °C of reaction temperature for 3 h. The predicted and experimental biodiesel yields under these reaction conditions were 89.42 and 89.40%, which showing less than 0.05% variation. Additionally, optimum biodiesel yield can be predicted by drawing 3D surface plots and 2D contour plots using MINITAB 17 software. For the characterization of the obtained biodiesel, analysis including the GC/MS, FT-IR, 1H NMR and 13C NMR were applied. The fuel properties of obtained biodiesel agrees well with the different European Union (EU-14214), China (GB/T 20828), and American (ASTM-951, 6751) standards.
This work incorporated technological values into Zn2Cr-layered double hydroxide (LDH), synthesized from unused resources, for removal of pyrophosphate (PP) in electroplating wastewater. To adopt a resource recovery for the remediation of the aquatic environment, the Zn2Cr-LDH was fabricated by co-precipitation from concentrated metals of plating waste that remained as industrial by-products from metal finishing processes. To examine its applicability for water treatment, batch experiments were conducted at optimum M2+/M3+, pH, reaction time, and temperature. To understand the adsorption mechanisms of the PP by the adsorbent, the Zn2Cr-LDH was characterized using Brunauer-Emmett-Teller (BET), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analyses before and after adsorption treatment. An almost complete PP removal was attained by the Zn2Cr-LDH at optimized conditions: 50 mg/L of PP, 1 g/L of adsorbent, pH 6, and 6 h of reaction. Ion exchange controlled the PP removal by the adsorbent at acidic conditions. The PP removal well fitted a pseudo-second-order kinetics and/or the Langmuir isotherm model with 79 mg/g of PP adsorption capacity. The spent Zn2Cr-LDH was regenerated with NaOH with 86% of efficiency for the first cycle. The treated effluents could comply with the discharge limit of <1 mg/L. Overall, the use of the Zn2Cr-LDH as a low-cost adsorbent for wastewater treatment has contributed to national policy that promotes a zero-waste approach for a circular economy (CE) through a resource recovery paradigm.
Iron-doped titanium dioxide loaded on activated carbon (Fe-TiO2/AC) was successfully synthesized from oil palm empty fruit bunch (OPEFB) using sol-gel method. The properties of the synthesized pure TiO2, Fe-doped TiO2, AC, TiO2/AC and Fe-TiO2/AC were examined by various techniques such as field emission scanning electron microscopy (FE-SEM), Fourier-transform infrared spectroscopy (FT-IR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) and nitrogen adsorption-desorption analyses at 77 K. FE-SEM revealed that Fe-doped TiO2 particles were dispersed homogeneously on the AC surface. FT-IR demonstrated high surface hydroxylation after Fe doping on TiO2 and UV-Vis DRS showed that Fe-TiO2/AC had the lowest band gap energy. Catalytic performance results proved that Fe dopants could restrict the recombination rate of hole and electron pairs, whereas AC support improved the Malachite Green (MG) adsorption sites and active sites of the hybrid catalyst. Photocatalytic degradation of 100 mg/L MG in the presence of 1.0 g/L 15 wt% Fe-TiO2 incorporated with 25 wt% AC, initial solution pH of 4 and 3 mM H2O2 could achieve the highest removal efficiency of 97% after 45 min light irradiation. This work demonstrates a promising approach to synthesis an inexpensive and efficient Fe-TiO2/AC for the photocatalytic degradation of organic dye.
The lack of aesthetic properties of electrospun nanofibres in terms of colour appearance is the drive in this preliminary study. This research is conducted to study the dyeing behaviour and colorimetric properties of electrospun nanofibres blended with Remazol Yellow FG reactive dye using dope-dyeing method via electrospinning process. This paper reports the colorimetric properties of dyed poly vinyl alcohol (PVA) nanofibres within the range of 2.5 wt.% to 12.5 wt.% dye content. The electrospinning parameters were fixed at the electrospinning distance of 10 cm, constant feed rate of 0.5 mL/h and applied voltage of 15 kV. The resulting impregnated dye of 10 wt.% exhibits acceptable colour difference of dyed PVA nanofibres, with a mean fibre diameter of 177.1 ± 11.5 nm. The SEM micrographs show the effect of dye content on morphology and fibre diameter upon the increment of dye used. Further increase of dye content adversely affects the jet stability during the electrospinning, resulting in macroscopic dropping phenomenon. The presence of all prominent peaks of Remazol dye in the PVA nanofibers was supported with FTIR analysis. The addition of dye into the nanofibres has resulted in the enhancement of thermal stability of the PVA as demonstrated by TGA analysis.
In this study, activated carbon (AC) was prepared from agro-waste betel nut husks (BNH) through the chemical activation method. Different characterization techniques described the physicochemical nature of betel nut husks activated carbon (BNH-AC) through Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), and pH point of zero charge. Later, the produced AC was used for methylene blue (MB) adsorption via numerous batch experimental parameters: initial concentrations of MB dye (25-250 mg/L), contact time (0.5-24 hours) and initial pH (2-12). Dye adsorption isotherms were also assessed at three temperatures where the maximum adsorption capacity (381.6 mg/g) was found at 30 °C. The adsorption equilibrium data were best suited to the non-linear form of the Freundlich isotherm model. Additionally, non-linear pseudo-second-order kinetic model was better fitted with the experimental value as well. Steady motion of solute particles from the boundary layer to the BNH-AC's surface was the possible reaction dynamics concerning MB adsorption. Thermodynamic study revealed that the adsorption process was spontaneous and exothermic in nature. Saline water emerged as an efficient eluent for the desorption of adsorbed dye on AC. Therefore, the BNH-AC is a very promising and cost-effective adsorbent for MB dye treatment and has high adsorption capacity.
A novel nanocomposite of MGO-NGC, composed of magnetic Fe3O4 nanoparticles (M), graphene oxide (GO), and N-methyl-d-glucamine functionalized calix[4]arene (NGC), was synthesized and applied as an effective adsorbent for the removal of two selected pesticides, namely hexaconazole and chlorpyrifos from water samples. The adsorbent was characterized by FTIR, SEM, EDX, TEM, and XRD. The main parameters affecting the adsorption process such as adsorbent dosage, pH of sample solution, salt effect, pesticide concentration, and adsorption time were investigated. The data from kinetic studies fitted well to the pseudo-second order kinetic model with R2 > 0.99. Among the isotherm models of Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich, the Langmuir isotherm fitted well to the adsorption process and demonstrated the monolayer adsorption pattern of the pesticides. Moreover, high adsorption capacities of 78.74 and 93.46 mg g-1 were obtained for chlorpyrifos and hexaconazole, respectively. Thermodynamic and free energy data indicated the physisorption mechanism for the adsorption process. The new adsorbent can be employed as an efficient, environment friendly, and highly reusable alternative for the removal of chlorinated pesticides from aqueous media.
Phytochemical study was conducted on the leaves of Globimetula braunii which is a hemi parasitic plant belonging to the family Loranthaceae. Extraction was carried out using cold extraction method with increasing polarity of solvents i.e n-hexane, CH2Cl2 and MeOH. The components were separated by chromatographic technique and the structures of the compounds were elucidated by extensive spectroscopic analyses including MS, FTIR, 1D and 2D NMR, HRMS and chemical methods. Six new pentacyclic triterpenoid esters named as globrauneine A (1), globrauneine B (2), globrauneine C (3), globrauneine D (4), globrauneine E (5), and globrauneine F (6), together with six known compounds (7 - 12) were successfully isolated from the leaves of G. braunii growing on Piliostigma thonningii. These results depict a substantial support to the chemotaxonomy of the genus Globimetula.
Cardiovascular application of nanomaterial's is of increasing demand and its usage is limited by its mechanical and blood compatible properties. In this work, an attempt is made to develop an electrospun novel nanocomposite loaded with basil oil and titanium dioxide (TiO2) particles. The composite material displayed increase in hydrophobic and reduced fiber diameter compared to the pristine polymer. Fourier transform infrared spectroscopy results showed the interaction of the pristine polymer with the added substances. Thermal analysis showed the increased onset degradation, whereas the mechanical testing portrayed the increased tensile strength of the composites. Finally, the composite delayed the coagulation times and also rendered safe environment for red blood cells signifying its suitability to be used in contact with blood. Strikingly, the cellular toxicity of the developed composite was lower than the pristine polymer suggesting its compatible nature with the surrounding tissues. With these promising characteristics, developed material with enhanced physicochemical properties and blood compatibility can be successfully utilized for cardiac tissue applications.
Due to the outbreak of the COVID-19 pandemic, practicing personal hygiene such as frequent hand sanitising has become a norm. The making of effective hand sanitiser products should follow the recommended formulations, but the high demand worldwide for such affordable products could have made them a candidate for counterfeiting, thus deserving forensic determination and profiling for source determination or supply chain tracing. In this study, determination and discrimination of hand sanitisers was carried out by employing attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy combined with chemometrics. Fifty commercially available hand sanitisers were obtained from the market and analysed. ATR-FTIR profiles of each sanitiser were compared and decomposed by principal component analysis (PCA) followed by linear discriminant analysis (LDA). Physical observation enabled the discrimination of seven samples based on their respective colours, the presence of beads and their colours, and the physical forms of formulations. Subsequently, eight distinct patterns were observed through visual comparison of ATR-FTIR profiles of the remaining 43 samples. An initial unsupervised exploratory PCA model indicated the separation of two main groups with ATR-FTIR profiles similar to those of ethanol and isopropanol, respectively. The PCA score-LDA model provided good predictions, with a 100% correct classification into eight different groups. In conclusion, this study demonstrated a quick determination and discrimination of hand sanitiser samples, allowing screening for any restricted components and sample-to-sample comparison.
Crude jatropha oil (JO) was modified to form jatropha oil-based polyol (JOL) via two steps in a chemical reaction known as epoxidation and hydroxylation. JOL was then reacted with isocyanates to produce JO-based polyurethane resin. In this study, two types of isocyanates, 2,4-toluene diisocyanate (2,4-TDI) and isophorone diisocyanate (IPDI) were introduced to produce JPUA-TDI and JPUA-IPDI respectively. 2,4-TDI is categorised as an aromatic isocyanate whilst IPDI is known as a cycloaliphatic isocyanate. Both JPUA-TDI and JPUA-IPDI were then end-capped by the acrylate functional group of 2-hydroxyethyl methacrylate (HEMA). The effects of that isocyanate structure were investigated for their physico, chemical and thermal properties. The changes of the functional groups during each synthesis step were monitored by FTIR analysis. The appearance of urethane peaks was observed at 1532 cm-1, 1718 cm-1 and 3369 cm-1 while acrylate peaks were detected at 815 cm-1 and 1663 cm-1 indicating that JPUA was successfully synthesised. It was found that the molar mass of JPUA-TDI was doubled compared to JPUA-IPDI. Each resin showed a similar degradation pattern analysed by thermal gravimetric analysis (TGA). For the mechanical properties, the JPUA-IPDI-based coating formulation exhibited a higher hardness value but poor adhesion compared to the JPUA-TDI-based coating formulation. Both types of jatropha-based polyurethane acrylate may potentially be used in an ultraviolet (UV) curing system specifically for clear coat surface applications to replace dependency on petroleum-based chemicals.