Anion clay hydrotalcite MgA1C0 3 with a Mg/A1 molar ratio of 3:1 was synthesized by co-precipitation at room temperature and pressure. The physicochemical properties were evaluated using Powder X-Ray Diffraction (PXRD), Fourier Transform Infrared (FTIR) spectroscopy and Thermogravimetric Analysis (TGA). The efficacy of anion clay hydrotalcite in the removal ofCcf- from aqueous solutions was investigated with respect to contact time, initial concentration, pH, adsorbent dosage and temperature. The Cd2- removal increased with the increased in contact time, adsorbent dosage, pH and initial concentration. Adsorption decreases with increasing initial concentration and temperature, for which the latter is indicative of an exothermic process. The equilibrium adsorption capacity of MgA1C0 3 was evaluated using linear Langmuir and Freundlich isotherms with respect to the separation factor, RL.
Two functional food oils, namely extra virgin olive oil (EVOO) and virgin coconut oil (VCO) have been analyzed simultaneously using Fourier transform infrared (FTIR) spectroscopy. The performance of multivariate calibration of principle component regression (PCR) and partial least square regression (PLSR) was evaluated in order to give the best prediction model for such determination. FTIR spectra were treated with several treatments including mean centering (MC), derivatization, and standard normal variate (SNV) at the combined frequency regions of 3050 – 3000, 1660 – 1650, and 1200 – 900 cm-1. Based on its capability to give the highest values of coefficient of correlation (R) for the relationship between actual value of EVOO/VCO and FTIR predicted value together with the lowest values of root mean square error of calibration (RMSEC), PLSR with mean centered-first derivative spectra was chosen for simultaneous determination of EVOO and VCO. It can be concluded that FTIR spectroscopy combined with multivariate calibration of PLSR was successfully applied to simultaneously quantify EVOO and VCO with acceptable parameters.
This aim of this research is to investigate thermal stability of virgin coconut oil, (VCO) which was heated at 190°C upon 40 days storage as compared to extra virgin olive oil (EVOO). The changes in fatty acids composition through (GC), Fourier Transform Infrared (FTIR) spectra, iodine value (IV) and total phenolic content were determined throughout the period of study. Results from GC showed that there was significant changes (P
FTIR spectroscopy in combination with multivariate calibrations, i.e. partial least square (PLS) and principle component regression (PCR) was developed for quantitative analysis of cod liver oil (CLO) in binary mixture with corn oil (CO). The spectra of CLO, CO and their blends with certain concentrations were scanned using horizontal attenuated total reflectance (HATR) accessory at mid infrared (MIR) region of 4,000 – 650 cm-1. The optimal spectral treatments selected for calibration models were based on its ability to provide the highest values of coefficient of determination (R2) and the lowest values of root mean error of calibration (RMSEC). PLS was slightly well suited for quantitative analysis of CLO compared to PCR. FTIR spectroscopy in combination with multivariate calibration offers rapid, no excessive chemical reagent, and easy in operational to be applied for determination of CLO in binary mixture with other oils.
Some cortical bone specimens from the femurs of adult cows and sea coral of Porites species were studied by using Fourier Transform Infrared Spectroscopy, FTIR. Carbonate were shown to be present by indication of C-O stretch found between 1510-1410 cm -1 in both cortical bone and Porites. Based on the comparison of the relative intensity of CO3 2- bands with respect to the PO4 3- bands, peak intensity of Porites was found to be higher than peak intensity of cortical bone at carbonate band. This explains that Porites skeleton is made up of CaCO3 while bone consists of a mineral, hydroxyapatite Ca5(PO4)3OH with the present of carbonate ions, typically from 3 to 7 wt%.
UV curable coating formulation comprises urethane acrylate resin and nanosilica as filler were synthesized to develop UV curable inorganic organic hybrid composite (PUA). The surface of the nanosilica was chemically modified to improve its chemical interaction within the urethane acrylate matrix. The modification had been undertaken by applying vinyltrymetoxysilane (VTMOS) that acted as a coupling agent to produce organophilic silica shell (SIMA). The shell is linked to the silica via reaction with the surface silanol group of the silica. The disappearance of metoxy groups in VTMOS was demonstrated by FTIR spectrum. The percentage of silica particles in UV curable hybrid formulation were varied on 5%, 10%, 15%, 20% and 250% respectively. In this work, the formulation was applied on medium density fiber board (11/IDF) substrate and subsequent has been irradiated under UV light. Then, the coated MDF were characterized by several testing equipments (TGA, DSC, scratch tester, instron, SEM). From the result, we found that the addition of silica nanoparticles exhibit significant improvement in coating film properties as compared to film without silica nanoparticle includes significant improvement in its modulus and scratch resistance. This make them as promising coating candidate for MDF product. On the other hand, we also found that an increase of silica particle up to 25 wt%, the viscosity has increased rapidly indicates that it is not suitable for acrylate coating formulation due to disappearance of desired effect known as tixotrophy.
Chitosan was chemically modified with bulky structure, cis-5-norbornene-2, 3-dicarboxylic anhydride and the characteristic of this modified chitosan was studied. The resulting material was analyzed by FTIR, TGA, DSC, XRD and SEM to study the effect of N-acylation to the polysaccharide structure. FTIR results show that the anhydride monomer was successfully bound to amine group of chitosan. Thermal analysis of the modified structure provides the chitosan fibers with thermal stability while XRD and SEM show the lost of crystallinity of modified chitosan. XRD of modified chitosan shows broader peak pattern and a considerable increase in a dimension while SEM of chitosan presented the single particle morphology while norbornene-chitosan shows aggromolarate behaviour due to the hydrophobic nature of norbornene pendant group which induced aggromolaration of the particles in modified structure.
The study examined modified Fenton (FeGAC/H2O2) pretreatment of the antibiotics amoxicillin and cloxacillin in aqueous solution for biological treatment. The treatment was optimized by the response surface methodology (RSM). The optimum operating conditions at pH3 were H2O2/COD molar ratio 2.0, FeGAC dose 3.5 g/L and reaction time 90 min for 87.53% removal of COD, 78.01% removal of TOC, and 98.24% removal of NH3-N. Biodegradability (BOD5/COD ratio) improved from zero to 0.36, indicating the effluent was amenable to biological treatment. Meanwhile, FTIR spectra indicated degradation of the antibiotics. Compared with Fenton or photo-Fenton, modified Fenton (FeGAC/H2O2) was more effective in the pre-treatment of the antibiotics amoxicillin and cloxacillin in aqueous solution for biological treatment.
The aim of this work is to study the effect of hydrocolloids (guar gum, xanthan gum and carboxymethyl cellulose (CMC) on the physical properties and sensory evaluation of ice cream produced in order to investigate the potential of applying fermented glutinous rice (tapai pulut) as a value-added ingredient. The addition of 25% fermented glutinous rice was the most reliable amount to enhance the physical and sensory properties of ice cream when incorporating hydrocolloids. The addition of hydrocolloids significantly (p < 0.05) increased the pH, firmness, overrun, and melting rate of fermented glutinous rice ice cream. The addition of guar gum scored the highest firmness value (5403 g) followed by CMC (4630 g) and xanthan gum (3481g). Fermented glutinous rice ice cream with xanthan gum added, induced a noticeable change in overrun value (62%) while the addition of CMC decreased the melting rate compared to the control. The FTIR spectrum of fermented glutinous rice ice cream with different hydrocolloids containing carboxyl, amide and carbonyl group was appeared at 3362-3379 cm-1 , 1639-1640 cm-1 and 1026-1064 cm-1, respectively. In conclusion, the addition of xanthan gum presented great potential to improve the quality of fermented glutinous rice ice cream produced in terms of its firmness, overrun and melting rate.
This study was conducted to prepare a mixed matrix membrane (MMM) and to test the performance of the prepared MMM for CO2 and CH4 gas separation. MMM containing polyethersulfone (PES) and multi-walled carbon nanotubes (MWCNTs) was prepared by a dry-wet phase inversion technique using a pneumatically-controlled membrane casting machine. The surface modification was performed on MWCNTs in order to enhance the selectivity of CO2/CH4. The surface modification of MWCNTs using chemical and physical approaches has been adopted. Mixed acid (HNO3/H2SO4) and β-CD were used for chemical and physical approaches, respectively. Effects of surface modification on MWCNTs/PES MMM were investigated. MWCNTs/PES MMMs were characterised using scanning electron microscopy (SEM), the Fourier Transform Infrared (FT-IR) spectroscopy and pure gas permeation test. The permeability and selectivity, which are the parameters describing membrane performance were calculated via the data obtained from pure gas permeation test with the feed pressure difference from 3 to 7 bars. In this study, surface modified MWCNTs/PES MMM using mixed acid and β-CD has successfully enhanced the CO2/CH4 selectivity by 40.6% compared to that of neat PES.
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 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.
In this paper, the adsorptive performance of synthesized thiourea (TU) modified poly(acrylonitrile-co-acrylic acid) (TU-P(AN-co-AA)) polymeric adsorbent for capturing p-nitrophenol (PNP) from aqueous solution was investigated. TU-P(AN-co-AA) was synthesized via the redox polymerization method with acrylonitrile (AN) and acrylic acid (AA) as the monomers, then modified chemically with thiourea (TU). Characterization analysis with Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), elemental microanalysis for CHNS, zeta potential measurement, Brunauer-Emmett-Teller (BET) surface analysis and thermal analyses were carried out to determine the morphology and physico-chemical properties of the synthesized polymer. The characterization results indicated successful surface modification of polymer with TU. The performance of TU-P(AN-co-AA) for the removal of PNP was investigated under various experimental parameters (adsorbent dosage, initial adsorbate concentration, contact time and temperature). The results demonstrated that the Freundlich isotherm model and pseudo-second-order kinetic model best described the equilibrium and kinetic data, respectively. Thermodynamic studies showed that the uptake of PNP by TU-P(AN-co-AA) was spontaneous and exothermic in nature. The results of the regeneration studies suggested that the TU-P(AN-co-AA) polymer is a reusable adsorbent with great potential for removing PNP from wastewater.
Development of strategies for removing heavy metals from aquatic environments is in high demand. Cadmium is one of the most dangerous metals in the environment, even under extremely low quantities. In this study, kenaf and magnetic biochar composite were prepared for the adsorption of Cd2+. The synthesized biochar was characterized using (a vibrating-sample magnetometer VSM), Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). The adsorption batch study was carried out to investigate the influence of pH, kinetics, isotherm, and thermodynamics on Cd2+ adsorption. The characterization results demonstrated that the biochar contained iron particles that help in improving the textural properties (i.e., surface area and pore volume), increasing the number of oxygen-containing groups, and forming inner-sphere complexes with oxygen-containing groups. The adsorption study results show that optimum adsorption was achieved under pH 5-6. An increase in initial ion concentration and solution temperature resulted in increased adsorption capacity. Surface modification of biochar using iron oxide for imposing magnetic property allowed for easy separation by external magnet and regeneration. The magnetic biochar composite also showed a higher affinity to Cd2+ than the pristine biochar. The adsorption data fit well with the pseudo-second-order and the Langmuir isotherm, with the maximum adsorption capacity of 47.90 mg/g.
In this work, fibrous silica-titania (FST) was successfully prepared by the microemulsion method prior to the addition of three types of carbonaceous materials: graphitic-carbon nitride, g-C3N4 (CN), graphene nanoplatelets (GN), and multi-wall carbon nanotubes, MWCNT (CNT), via a solid-state microwave irradiation technique. The catalysts were characterized using XRD, FESEM, TEM, FTIR, UV-Vis DRS, N2 adsorption-desorption, XPS and ESR, while their photoactivity was examined on the degradation of toxic 2-chlorophenol (2-CP). The result demonstrated that the initial reaction rate was in the following order: CNFST (5.1 × 10-3 mM min-1) > GNFST (2.5 × 10-3 mM min-1) > CNTFST (2.3 × 10-3 mM min-1). The best performance was due to the polymeric structure of g-C3N4 with a good dispersion of C and N on the surface FST. This dispersion contributed towards an appropriate quantity of defect sites, as a consequence of the greater interaction between g-C3N4 and the FST support, that led to narrowed of band gap energy (2.98 eV to 2.10 eV). The effect of scavenger and ESR studies confirmed that the photodegradation over CNFST occurred via a Z-scheme mechanism. It is noteworthy that the addition of green carbonaceous materials on the FST markedly enhanced the photodegradation of toxic 2-CP.
Agglomeration and restacking can reduce graphene oxide (GO) activity in a wide range of applications. Herein, GO was synthesized by a modified Hummer's method. To minimize restacking and agglomeration, in situ chemical oxidation polymerization was carried out to embed polyaniline (PANI) chains at the edges of GO sheets, to obtain GO-PANI nanocomposite. The GO-PANI was tested for the adsorptive removal of brilliant green (BG) from an aqueous solution through batch mode studies. Infrared (FT-IR) analysis revealed the dominance of hydroxyl and carboxylic functionalities over the GO-PANI surface. Solution pH-dependent BG uptake was observed, with maximum adsorption at pH 7, and attaining equilibrium in 30 min. The adsorption of BG onto GO-PANI was fit to the Langmuir isotherm, and pseudo-second-order kinetic models, with a maximum monolayer adsorption capacity (qm) of 142.8 mg/g. An endothermic adsorption process was observed. Mechanistically, π-π stacking interaction and electrostatic interaction played a critical role during BG adsorption on GO-PANI.
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.
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.
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.
Soda lime silica (SLS) waste as the source of silica (SiO2) and ark clamshell (ACS) as the foaming agent has been utilized to fabricate the low-cost and lightweight foam glass-ceramics. A series of 1 and 6 wt% foam glass-ceramics were successfully prepared by the conventional solid-state sintering method at various sintering temperatures for 60 min. The bulk density of the samples has achieved minimum density (1.014 g/cm3) with maximum expansion (62.31%) at 6 wt% of the ACS content sintered at 800 °C for 60 min. The bulk density increases while the linear shrinkage and total porosity decrease with the progression of ACS contents and sintering temperature, where the results correspond with the FESEM micrograph. The result of XRD and FTIR transmittance spectra have shown that the formation of wollastonite crystal has occurred starting at 6 wt% of the ACS content sintered at 800 °C for 30 min. The highest mechanical performance (3.90 MPa) with an average total porosity (8.04%) is observed for the sample containing 1 wt% of ACS. It can be concluded that the composition of foam glass-ceramics (1 and 6 wt%) and sintering temperatures give significant results to the structural, physical, and mechanical properties of the fabricated foam glass-ceramics.