In this work, polymer electrolytes have been prepared by doping starch with Sodium Phosphate (Na3PO4). The incorporation of 25% Na3PO4 optimizes the room temperature conductivity of the electrolyte at 7.27 x 10-6 Scm-1. The temperature dependence of conductivity for the electrolyte is Arrhenius and the activation energy, Ea, of 75% corn starch-25% Na3PO4 electrolyte is 0.26eV. The dielectric studies reveal the non-Debye nature of the electrolyte. The complexation of Na3PO4 with the polymer host was studied using Fourier transform infrared (FTIR) spectroscopy.
Magnetic nanocomposites adorned with calixarene were successfully prepared by immobilizing diethanolamine functionalized p-tert-butylcalix[4]arene (DEA-Calix) onto silica-coated magnetic nanoparticles (MNPs). The synthesis, surface morphology, purity, elemental composition and thermal stability of newly prepared nanocomposites were analyzed using FT-IR spectroscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX), X-ray diffractometer (XRD), thermal gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Magnetic solid-phase adsorption (MSPA) was employed to explore the adsorption behavior of DEA-Calix-MNPs towards Pb(II) from water samples prior to its flame atomic absorption spectrometric analysis. The essential analytical factors governing the adsorption efficiency such as solution pH, mass of adsorbent, concentration and contact time have been investigated and optimized. The results depict that DEA-Calix-MNPs has excellent adsorption efficiency 97% (at pH 5.5) with high adsorption capacity of 51.81 mg g-1 for Pb(II) adsorption. Additionally, kinetic and equilibrium studies suggested that Pb(II) adsorption process follows a pseudo-second-order model and Langmuir isotherms, respectively. Real sample analysis also confirmed field applicability of the new DEA-Calix-MNPs adsorbent.
A series of glass samples with chemical formula {[(TeO2)0.7(B2O3)0.3]0.7(ZnO)0.3}1-x(Dy2O3)xwhere x=0.01, 0.02, 0.03, 0.04 and 0.05M fraction were synthesized through conventional melt-quenching method. The most common way to fabricate a glass material is by fusion of two or more component oxides followed by their quenching. This technique is known as melt-quenching technique. Kaur et al. (2016) [1] highlighted that the melt-quenching method able to enhance the mechanical properties like hardness and flexural strength of the material. The nature of the glass systems is proven to be amorphous based on the XRD pattern. The FTIR spectra of the glass systems confirm the existence of five bands which are assigned for the BO4, BO3,TeO4and TeO3vibrational groups. The density of the glass systems is increased with the addition of Dy2O3while the molar volume is found to be inversely proportional to the density of the proposed glass. The optical properties of the glasses are determined through the absorption spectra obtained from the UV-VIS spectrophotometer. From the absorption spectra, the indirect and direct optical band gaps and the Urbach energy are found to be inversely proportional to each other. As the molar fraction of the Dy2O3increased, the optical band gaps are observed to increase as opposed to the Urbach energy. For this glass system, the values of refractive index, electronic polarizability, oxide ion polarizability and the optical basicity are found to decrease as the addition of the dysprosium oxide is increased. From the emission spectra, two intense blue and yellow emission bands are observed, which correspond to the4F9/2→6H15/2and4F9/2→6H13/2transitions of Dy3+ions respectively. The CIE chromaticity coordinates of the zinc borotellurite glass systems are found to be located in the white light region.
The roles of multi-walled carbon nanotubes (MWNTs) and functionalised multiwalled carbon nanotubes (fMWNTs) in enhancing the efficacy of urea fertilizer (UF) as plant nutrition for local MR219 paddy variety was investigated. The MWNTs and fMWNTs were grafted onto UF to produce UF-MWNTs fertilizer with three different conditions, coded as FMU1 (0.6 wt. % fMWNTs), FMU2 (0.1 wt. % fMWNTs) and MU (0.6 wt. % MWNTs. The batches of MR219 paddy were systematically grown in accordance to the general practice performed by the Malaysian Agricultural Research and Development Institute (MARDI). The procedure was conducted using a pot under exposure to natural light at three different fertilization times; after a certain number of days of sowing (DAS) at 14, 35 and 55 days. Interestingly, it was found that the crop growth of plants treated with FMU1 and FMU2 significantly increased by 22.6% and 38.5% compared to plants with MU addition. Also, paddy treated with FMU1 produced 21.4% higher number of panicles and 35% more grain yield than MU while paddy treated with FMU2 gave 28.6% more number of panicles and 36% higher grain yield than MU, which implies the advantage of fMWNTs over MWNTs to be combined with UF as plant nutrition. The chemical composition and morphology of UF-MWNTs fertilizers which is further characterised by FTiR and FESEM confirmed the successful and homogeneous grafting of UF onto the fMWNTs.
Membrane technologies have received high interest in the separation gas mixture. The
ceramic inorganic membranes have possessed high permeability, excellent thermal,
chemical and mechanical stabilities compared to conventional polymer membranes.
This work presents the fabrication of silica ceramic membrane by sol dip-coating
method. The tubular support was dipped into the solution of tetrethylorthosilicate
(TEOS), distilled water and ethanol with the addition of nitric acid as a catalyst. The
fabricated silica membrane was then characterized by (Field Emission Scanning
Electron Microscope) FESEM and (Fourier transform infrared spectroscopy) FTIR to
determine structural and chemical properties at different dipping number. FESEM
images indicate that the silica has been deposited on the surface fabricated ceramic
membrane and penetrate into the pore walls. However, number of dipping did not
affect the intensity peak of FTIR analysis.
Microplastics (MPs) are generated from plastic and have negative impact to our environment due to high level of fragmentation. They can be originated from various sources in different forms such as fragment, fiber, foam and so on. For detection of MPs, many techniques have been developed with different functions such as microscopic observation, density separation, Raman and FTIR analysis. Besides, due to ingestion of MPs by wide range of marine species, research on the effect of this pollution on biota as well as human is vital. Therefore, we comprehensively reviewed the occurrence and distribution of MPs pollution in both marine and freshwater environments, including rivers, lakes and wastewater treatment plants (WWTPs). For future studies, we propose the development of new techniques for sampling MPs in aquatic environments and biota and recommend more research regarding MPs release by WWTPs.
In the present study, we attempted revalorization of pear (Pyrus pyrifolia L.) peel residue into high value-added nanomaterials. A green and facile one-pot isolation procedure was designed to simplify the isolation process of nanocellulose directly from pear peel residue. The one-pot approach employed in this work is interesting as the reaction involved less harmful chemicals usage and non-multiple steps. The reaction was carried out by adding hydrogen peroxide as an oxidant and chromium (III) nitrate as catalyst in the acidic medium under mild process conditions. FTIR spectroscopy proved that the pear peel derived nanocellulose was purely cellulose phases without the presence of non-cellulosic layer. XRD study indicated that the isolated nanocellulose possessed of cellulose I polymorph with high crystallinity index of 85.7%. FESEM analysis clearly revealed that the considerable size reduction during one-pot process. Remarkably, TEM analysis revealed that the isolated nanocellulose consisted of network-liked nature and spherical shaped morphologies with high aspect ratio of 24.6. TGA showed nanocellulose has lower thermal stability compared to pear peel residue. This study provided a cost-effective method and straightforward one-pot process for fabrication of nanocellulose from pear peel residue. This is the first investigation on the nanocellulose extraction from pear fruit.
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.
Nanofibrillated cellulose (NFCs) were extracted from sugar palm fibres (SPS) in two separate stages; delignification and mercerization to remove lignin and hemicellulose, respectively. Subsequently, the obtained cellulose fibres were then mechanically extracted into nanofibres using high pressurized homogenization (HPH). The diameter distribution sizes of the isolated nanofibres were dependent on the cycle number of HPH treatment. TEM micro-images displayed the decreasing trend of NFCs diameter, from 21.37 to 5.5 nm when the number of cycle HPH was increased from 5 to 15 cycles, meanwhile TGA and XRD analysis showed that the degradation temperature and crystallinity of the NFCs were slightly increased from 347 to 347.3 °C and 75.38 to 81.19% respectively, when the number of cycles increased. Others analysis also were carried on such as FT-IR, FESEM, AFM, physical properties, zeta potential and yield analysis. The isolated NFCs may be potentially applied in various application, such as tissue engineering scaffolds, bio-nanocomposites, filtration media, bio-packaging and etc.
Titanium dioxide nanoparticles were synthesized by using sol gel method and their physico-chemical properties were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and UV-Vis spectrophotometer. The photocatalytic property of TiO2 nanoparticles was investigated by inactivation of Escherichia coli under irradiation of fluorescent lamp. The results showed that the size of TiO2 was in the range of 3 to 7 nm with high crystallinity of anatase phase. The sharp peaks in FTIR spectrum determined the purity of TiO2 nanoparticles and absorbance peak of UV-Vis spectrum showed the energy band gap of 3.2 eV. Optimum inactivation of E. coli was obtained at 1.0 g/L TiO2 nanoparticles, with 80% of E. coli population was inactivated. The light scattering effect and insufficient concentration are the factors that cause the less effective inactivation reaction for 2.5 g/L and 0.1 g/L TiO2 concentration.
The effects of rf power on the structural properties of hydrogenated nanocrystalline silicon (nc-Si:H) thin films deposited using layer-by-layer (LbL) deposition technique in a home-built plasma enhanced chemical vapor deposition (PECVD) system were investigated. The properties of the films were characterized by X-ray diffraction (XRD), microRaman scattering spectroscopy, high resolution transmission electron microscope (HRTEM) and Fourier transform infrared (FTIR) spectroscopy. The results showed that the films consisted of different size of Si crystallites embedded within an amorphous matrix and the growth of these crystallites was suppressed at higher rf powers. The crystalline volume fraction of the films was optimum at the rf power of 60 W and contained both small and big crystallites
with diameters of 3.7 nm and 120 nm, respectively. The hydrogen content increased with increasing rf power and enhanced the structural disorder of the amorphous matrix thus decreasing the crystalline volume fraction of the films. Correlation of crystalline volume fraction, hydrogen content and structure disorder of the films under the effect of rf
power is discussed.
The fractions of fatty acid methyl esters (FAME) i.e. crude palm oil methyl esters (CPOME), RBD palm olein methyl esters (RBD Palm Olein ME) and used frying oil methyl esters (UFOME) rich in unsaturated fatty esters were used to prepare alkenyl succinic anhydrides (ASA). The fractions were obtained via fractional distillation that separated the unsaturated fatty esters from the saturated fatty esters. The fractions with the highest content of unsaturated fatty esters were reacted with maleic anhydride (MA) for 8 hours at 240oC with the MA/FAME ratio of 1.5. The reaction was conducted without catalyst and solvent. The crude alkenyl succinic anhydride (ASA) obtained was purified by column chromatography. The purified compound was characterised by FTIR.
Surface modification of rice husk (RH) with alkali pre-treatment (NaOH solution 5% w/v) was carried out at the initial state to investigate the effect of surface treatment of fibre on the surface interaction between fibre and rubber. Further modification of RH surfaces after alkali treatment was using Liquid Epoxidized Natural Rubber (LENR) coating at three concentrations, 5%, 10%, and 20% wt LENR solution in toluene. Interfacial morphology and chemical reactions between RH fibre and rubber were analyzed by FTIR and Scanning Electron Microscope (SEM). It was found that 10% wt LENR solution gave the optimum interaction between fibre and rubber. Matrix and composite blends derived from 60% natural rubber (NR), 40% high density polyethylene (HDPE) reinforced with RH fibre were prepared using an internal mixer (Brabender Plasticoder). Result showed that pre-treatment of RH treated with 5% NaOH followed by treatment with 10% LENR solution given the maximum interaction between fibre and matrix that gave rise to better mechanical properties of the composites.
A new heterocyclic coupling agent has been produced from the reaction of maleic anhydride and p-aminophenol, namely N-(4-hydroxylpheneyl)maleimide. The coupling agent underwent azo coupling reaction with aromatic amine, which is p-aminophenol to produce a new heterocyclic azo pigment. The pigment was then subjected to solubility, hiding power and light fastness test. Fourier Transform Infrared Spectroscopy (FTIR), Ultraviolet/Visible (UV/Vis) Spectroscopy, and Nuclear Magnetic Resonance Spectroscopy (1H-NMR, 13C-NMR) were used to obtain the characteristics and structural features of the pigment.
In-situ polymerization method was used to prepare palm-based polyurethane (PU) composites loading with 15 wt% magnetite (Fe3O4), polyaniline (PANI) and Fe3O4 coated with PANI labeled as PU15, PP and PPM, respectively. FTIR spectroscopy analysis indicated a shift in the carbonyl, C=O and NH in PP. The shift of the peak indicated that there was hydrogen bonding between the C=O (proton acceptor) of urethane with NH (proton-donator) of PANI. PPM gave the highest impact and flexural strengths at 4875 kJ/ m2 and 42 MPa, respectively but with the lowest flexural modulus (1050 MPa). Two-stage degradation behavior was observed in the TGA thermogram.
A series of poly(urea-formaldehyde) (PUF) microcapsules filled with dicyclopentadiene (DCPD) was successfully prepared by in situ polymerization. The effect of diverse process parameters and ingredients on the morphology of the microcapsules was observed by SEM, optical microscopy (OM) and digital microscopy. Different techniques for the characterization of the chemical structure and the core content were considered such as FT-IR and 1H-NMR as well as the characterization of thermal properties by DSC. High yields of free flowing powder of spherical microcapsules were produced. The synthesized microcapsules can be incorporated into another polymeric host material. In the event the host material cracks due to excessive stress or strong impact, the microcapsules would rupture to release the DCPD, which could polymerize to repair the crack.
Different type of fibers which is EFB and KC were liquefied in phenol with the presence of sulphuric acid as a catalyst. The liquefied residue was characterized by using Fourier transform infrared (FTIR) to determine the functional groups presents in both residues, X-ray diffraction (XRD) to determine the degree of crystallinity in the residue, thermogravimetric analysis (TGA) to analyze the thermal properties of the residue and scanning electron microscope (SEM) to investigate the structure and morphology of the residue. Phenol-to-EFB/KC ratio shows great effect on the amount of residue in the liquefaction process. Peak appearance can be observed in the FTIR analysis at 810 and 750 cm-1 which is attributed to the para and meta benzene, respectively or to be specific its associated to the p-alkyl phenol and m-alkyl phenol. In the XRD analysis, CrI of lignocellulosic materials increased after liquefaction process. Liquefaction process caused chemical penetration across the grain of the fiber, thus the fiber bundles started to separate into individual fibers shown in the SEM micrograph and the weights lost curve for both liquefied EFB and KC experienced three region decompositions.
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.
In response to our review paper [L. C. Lee et al., Analyst, 2018, 143, 3526-3539], we present a study that compares empirical differences between PLS1-DA and PLS2-DA algorithms in modelling a colossal ATR-FTIR spectral dataset. Over the past two decades, partial least squares-discriminant analysis (PLS-DA) has gained wide acceptance and huge popularity in the field of applied research, partly due to its dimensionality reduction capability and ability to handle multicollinear and correlated variables. To solve a K-class problem (K > 2) using PLS-DA and high-dimensional data like infrared spectra, one can construct either K one-versus-all PLS1-DA models or only one PLS2-DA model. The aim of this work is to explore empirical differences between the two PLS-DA algorithms in modeling a colossal ATR-FTIR spectral dataset. The practical task is to build a prediction model using the imbalanced, high dimensional, colossal and multi-class ATR-FTIR spectra of blue gel pen inks. Four different sub-datasets were prepared from the principal dataset by considering the raw and asymmetric least squares (AsLS) preprocessed forms: (a) Raw-global region; (b) Raw-local region; (c) AsLS-global region; and (d) AsLS-local region. A series of 50 models which includes the first 50 PLS components incrementally was constructed repeatedly using the four sub-datasets. Each model was evaluated using six different variants of v-fold cross validation, autoprediction and external testing methods. As a result, each PLS-DA algorithm was represented by a number of figures of merit. The differences between PLS1-DA and PLS2-DA algorithms were assessed using hypothesis tests with respect to model accuracy, stability and fitting. On the other hand, confusion matrices of the two PLS-DA algorithms were inspected carefully for assessment of model parsimony. Overall, both the algorithms presented satisfactory model accuracy and stability. Nonetheless, PLS1-DA models showed significantly higher accuracy rates than PLS2-DA models, whereas PLS2-DA models seem to be much more stable compared to PLS1-DA models. Eventually, PLS2-DA also proved to be less prone to overfitting and is more parsimonious than PLS1-DA. In conclusion, the relatively high accuracy of the PLS1-DA algorithm is achieved at the cost of rather low parsimony and stability, and with an increased risk of overfitting.
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.