The data in this article provide information on spectroscopic and theoretical data for p-chlorocalix[4]arene when combined with selected drugs, such as paracetamol, ibuprofen, and cetirizine. The present spectroscopic data are generated from Fourier Transform Infrared (FTIR), Nuclear Magnetic Resonance (1H NMR and 13C NMR), and Ultraviolet-Visible spectroscopy (UV-Vis) as the key tools for molecular characterization. The measurement of the optimization energy, interaction energy, and the band gap energy between the molecules was calculated by Gaussian 09 software. It is interesting to note that of the three titled drugs identified, p-chlorocalix[4]arene showed the highest interaction energy with paracetamol, followed by ibuprofen and cetirizine.
Oil palm empty fruit bunch (OPEFB) fiber/polylactic acid (PLA)-based composites filled with 6-22 wt.% multi-walled carbon nanotubes (MWCNTs) were prepared using a melt blend method. The composites were analyzed using X-ray diffraction (XRD), Fourier transforms infrared (FTIR), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) of the MWCNTs. The composites were characterized for complex permittivity using the coaxial probe at 8-12 GHz range and the transmission/reflection coefficients were measured through micro strip line. The dielectric permittivity measurements carried out at X-band frequency revealed that 22 wt.% MWCNTs nanocomposite display higher dielectric constant (ε') and dielectric loss (ε″) values of 4.23 and 0.65, respectively. A maximum absorption loss of 15.2 dB was obtained for the 22 wt.% nanocomposites at 11.75 GHz. This result suggests that PLA/OPEFB/MWCNTs composites are a promising cheap and lightweight material for the effective microwave absorption in the X-band frequency range.
Liquid natural rubber (LNR) was functionalized into liquid epoxidized natural rubber (LENR) and hydroxylated LNR (LNROH)
via oxidation using a Na2
WO4
/CH3
COOH/H2
O2
catalytic system. Microstructures of LNR and functionalized LNRs
were characterized using Fourier Transform Infrared (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopies. The
effect of CH3
COOH, H2
O2
, Na2
WO4
, reaction time and temperature. reaction time and temperature on epoxy content were
investigated. LNR-OH was obtained when oxidation reaction was conducted at a longer reaction time, higher temperature
or excess amount of catalyst. Thermogravimetric analysis (TGA) reported the thermal behavior of functionalized LNRs.
Molecular weight and polydispersity index (PDI) were determined using gel permeation chromatography (GPC).
Abuse of solvent-based adhesives jeopardizes world population, especially the young generation. Adhesive-related exhibits encountered in forensic cases might need to be determined if they could have come from a particular source or to establish link between cases or persons. This study was aimed to discriminate solvent-based adhesives, especially to aid forensic investigation of glue sniffing activities. In this study, thirteen brands with three samples each, totaling at 39 adhesive samples, were analyzed using attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy followed by chemometric methods. Experimental output showed that adhesive samples utilized in this study were less likely to change in their ATR-FTIR profiles over time, at least up to 2 months. No interference from plastic materials was noticed based on ATR-FTIR profile comparison. Physical examination could differentiate the samples into two groups, namely contact adhesives and cement adhesives. A principal component analysis-score linear discriminative analysis (PC-score LDA) model resulted in 100% and 98.6% correct classification in discriminating the two groups of adhesive samples, forming seven discriminative clusters. Test set with adhesive samples applied glass slide and plastic substrates also demonstrated a 100% correct classification into their respective groups. As a conclusion, the method allowed for discrimination of adhesive samples based on the spectral features, displaying relationship among samples. It is hoped that this comparative information is beneficial to trace the possible source of solvent-based adhesives, whenever they are recovered from a crime scene, for forensic investigation.
Extra virgin olive oil (EVOO) is categorized as expensive oil due to high-quality nutritional value. Unfortunately, EVOO is easily adulterated with other low-quality edible oils. Therefore, this study was done to differentiate and analyze the adulteration of EVOO with other edible oils using Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectroscopy. The study was used several edible oils included canola oil, corn oil, sunflower oil, and soybean oil as an adulterant for EVOO. The adulterant EVOO samples were prepared by mixing with dissimilar concentrations of the solely edible oils (20 %, 40 %, 60 % and 80 % (v/v)). The main functional groups of EVOO and other edible oils are O-H, C-H, C=C and C=O groups were assigned around 3500 cm-1, 2925 cm-1, 3006 cm-1 and 1745 cm-1 wavenumbers, respectively. From the comparison of EVOO and other adulterant edibles oil spectra, it showed that the EVOO has the lowest absorbance intensity at around 3006 cm-1 represented double bond which is closely related to the composition of oil sample. The adulteration of EVOO was evaluated by analysing the changes in the absorbance based on the linear regression analysis graph of the bands at 3006 and 2925 cm-1 and the limit of detection (LOD) was measured. The graph of A3008/A2925 with good relative coefficients (R2) and lower LOD is more favourable than the linear regression graph of A3006 versus percentage of edible oils added in EVOO. This study showed that ATR-FTIR spectroscopy is a convenient tool for analysing the adulteration of EVOO.
The hydrophobic membranes have been widely explored to meet the membrane characteristics for the membrane distillation (MD) process. Inorganic metal oxide nanoparticles have been used to improve the membrane hydrophobicity, but limited studies have used nano clay particles. This study introduces halloysite nanotube (HNT) as an alternative material to synthesis a hydrophobic poly(vinylidene fluoride) (PVDF)-HNT membrane. The PVDF membranes were fabricated using functionalized HNTs (e.g., carnauba wax and 1H,1H,2H,2H-perfluorooctyl-trichlorosilane (FOTS)). The results were determined by Fourier transform infrared-attenuated total reflection, scanning electron microscope, goniometer and porometer to determine the desired hydrophobic membrane for direct contact membrane distillation (DCMD). The addition of FOTS-HNT (fs-HNT) and carnauba wax-HNT (fw-HNT) in the PVDF membrane enhanced the water contact angle (CA) to 127° and 137°, respectively. The presence of fw-HNT in the PVDF membrane exhibited higher liquid entry pressure (LEP) (2.64 bar) compared to fs-HNT in the membrane matrix (1.44 bar). The PVDF/fw-HNT membrane (Pfw-HNT) obtained the highest flux of 7.24 L/m2h with 99.9% salt removal. A stable permeability in the Pfw-HNT membrane was obtained throughout 16 h of DCMD. The incorporation of fw-HNT in the PVDF membrane had improved the anti-wetting properties and the membrane performance with the anti-fouling effect.
Introduction: Accelerants and fabrics are commonly used to spread fire attributable to their highly flammable prop- erties. Hence, having the ability to discriminate the different types of accelerants on various types of fabrics after fire and/or arson using the non-destructive Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spec- troscopy coupled with chemometric techniques appears forensically relevant. Methods: Six types of fabrics viz. cotton, wool, silk, rayon, satin, and polyester, were burnt completely with RON95 and RON97 gasoline as well as diesel. Subsequently, the samples were analyzed by ATR-FTIR spectroscopy followed by Principal Component Analysis (PCA) and Linear Discriminant Analysis (LDA) for discriminating the different types of accelerants on such burned fabrics. Results: RON95 showed the fastest rate of burning on all fabric types. Results also revealed that while wool had the slowest burning rate for all the three different accelerants, polyester, cotton, and satin demon- strated the highest rate of burning in RON95, RON97, and diesel, respectively. FTIR spectra revealed the presence of alkane, alcohol, alkene, alkyne, aromatic, and amine compounds for all fabrics. The two dimensional PCA (PC1 versus PC2) demonstrated 71% of variance and it was improved by cross-validation through the three dimensional LDA technique with correct classification of 77.8%. Conclusion: ATR-FTIR spectroscopy coupled with chemometric techniques had enabled identification of the functional groups, as well as statistically supported discrimination of the different accelerants, a matter of relevance in forensic fire and arson investigations.
Conocarpus fiber is an abundantly available and sustainable cellulosic biomass. With its richness in cellulose content, it is potentially used for manufacturing microcrystalline cellulose (MCC), a cellulose derivative product with versatile industrial applications. In this work, different samples of bleached fiber (CPBLH), alkali-treated fiber (CPAKL), and acid-treated fiber (CPMCC) were produced from Conocarpus through integrated chemical process of bleaching, alkaline cooking, and acid hydrolysis, respectively. Characterizations of samples were carried out with Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX), Fourier Transform Infrared-Ray (FTIR), X-ray Diffraction (XRD), Thermogravimetric (TGA), and Differential Scanning Calorimetry (DSC). From morphology study, the bundle fiber feature of CPBLH disintegrated into micro-size fibrils of CPMCC, showing the amorphous compounds were substantially removed through chemical depolymerization. Meanwhile, the elemental analysis also proved that the traces of impurities such as cations and anions were successfully eliminated from CPMCC. The CPMCC also gave a considerably high yield of 27%, which endowed it with great sustainability in acting as alternative biomass for MCC production. Physicochemical analysis revealed the existence of crystalline cellulose domain in CPMCC had contributed it 75.7% crystallinity. In thermal analysis, CPMCC had stable decomposition behavior comparing to CPBLH and CPAKL fibers. Therefore, Conocarpus fiber could be a promising candidate for extracting MCC with excellent properties in the future.
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.
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.
The structural, thermal, linear, and femtosecond third-order nonlinear optical (NLO) properties of two pyridine-based anthracene chalcones, (2E)-1-(anthracen-9-yl)-3-(pyridin-2-yl)prop-2-en-1-one (2PANC) and (2E)-1-(anthracen-9-yl)-3-(pyridin-3-yl)prop-2-en-1-one (3PANC), were investigated. These two chalcones were synthesized following the Claisen-Schmidt condensation method. Optically transparent single crystals were achieved using a slow evaporation solution growth technique. The presence of functional groups in these molecules was established by Fourier transform infrared and NMR spectroscopic data. The detailed solid-state structure of both chalcones was determined from the single-crystal X-ray diffraction data. Both crystals crystallized in the centrosymmetric triclinic space group P1̅ with the nuance of unit cell parameters. The crystals (labeled as 2PANC and 3PANC) have been found to be transparent optically [in the entire visible spectral region] and were found to be thermally stable up to 169 and 194 °C, respectively. The intermolecular interactions were investigated using the Hirshfeld surface analysis, and the band structures (highest occupied molecular orbital-lowest unoccupied molecular orbital, excited-state energies, global chemical reactivity descriptors, and molecular electrostatic potentials) were studied using density functional theory (DFT) techniques. The ultrafast third-order NLO properties were investigated using (a) Z-scan and (b) degenerate four-wave mixing (DFWM) techniques using ∼50 fs pulses at 800 nm (1 kHz, ∼4 mJ) from a Ti:sapphire laser amplifier. Two-photon-assisted reverse saturable absorption, self-focusing nonlinear refraction, optical limiting, and optical switching behaviors were witnessed from the Z-scan data. 3PANC demonstrated a stronger two-photon absorption coefficient, while 2PANC depicted a stronger nonlinear refractive index among the two. The time-resolved DFWM data demonstrated that the decay times of 2PANC and 3PANC were ∼162 and ∼180 fs, respectively. The second hyperpolarizability (γ) values determined by DFT, Z-scan, and DFWM were found to be in good correlation (with a magnitude of ∼10-34 esu). The ultrafast third-order NLO response, significant NLO properties, and thermal stability of these chalcones brands them as potential candidates for optical power limiting and switching applications.
Carbon nanoparticles have been widely used in various applications. However, they are commonly known to have low dispersibility and chemical inertness which limit their practical ability in medical or biological area. Some studies have been performed to modify carbon nanoparticles such as carbon nanotubes using ultraviolet (UV)-Ozone system. However, little is known on the effects of such system towards other types of carbon nanoparticles such as mesoporous hollow carbon nanoparticles (MHCNs). Thus, in this study, improvement of MHCNs physiochemical properties have been studied using UV-Ozone treatment for the first time. The treatment was conducted in water as dispersant agent at ozone flowrate of 1.0 L/min and exposure time of 45 min. SEM images observed that MHCNs morphology and surface structure remain intact after the treatment. Observations on the dispersibility of MHCNs in phosphate buffered saline (PBS) solution shows that the dispersibility was improved compared to the untreated ones. This was supported by the low Z-average and PDI values of treated MHCNs obtained at ~400 nm and 0.2, respectively when compared to the untreated MHCNs which was obtained at 970 nm and 0.417, respectively. Thermogravimetric analysis (TGA) showed an increased in weight loss of treated MHCNs at the lower temperature compared to untreated MHCNs. Results from Fourier Transform Infrared (FTIR) showed an increase number of new functional groups that includes carboxylic acid group presence at the surface of treated MHCNs which contributes to the improvement of their dispersibility, thermal properties and chemical functionality. These findings opened a new possibility of using UV-Ozone treatment to improve physicochemical properties of MHCNs for medical area such as in drug delivery application in addition to their excellent storage and carrier system.
This study investigated the engine performance and emission characteristics of biodiesel blends with combined Graphene oxide nanoplatelets (GNPs) and 10% v/v dimethyl carbonate (DMC) as fuel additives as well as analysed the tribological characteristics of those blends. 10% by volume DMC was mixed with 30% palm oil biodiesel blends with diesel. Three different concentrations (40, 80 and 120 ppm) of GNPs were added to these blends via the ultrasonication process to prepare the nanofuels. Sodium dodecyl sulphate (SDS) surfactant was added to improve the stability of these blends. GNPs were characterised using Scanning Electron Microscope (SEM) and Fourier Transform Infrared (FTIR), while the viscosity of nanofuels was investigated by rheometer. UV-spectrometry was used to determine the stability of these nanoplatelets. A ratio of 1:4 GNP: SDS was found to produce maximum stability in biodiesel. Performance and emissions characteristics of these nanofuels have been investigated in a four-stroke compression ignition engine. The maximum reduction in BSFC of 5.05% and the maximum BTE of 22.80% was for B30GNP40DMC10 compared to all other tested blends. A reduction in HC (25%) and CO (4.41%) were observed for B30DMC10, while a reduction in NOx of 3.65% was observed for B30GNP40DMC10. The diesel-biodiesel fuel blends with the addition of GNP exhibited a promising reduction in the average coefficient of friction 15.05%, 8.68% and 3.61% for 120, 80 and 40 ppm concentrations compared to B30. Thus, combined GNP and DMC showed excellent potential for utilisation in diesel engine operation.
Polymer had been widely used in industries nowadays. However, the properties of the polymer itself are limited to a particular application. This study describes synthetic clay, layered double hydroxide (LDH), as a filler in low-density polyethylene (LDPE) composite. LDHs of magnesium/aluminium-dodecyl sulfate (Mg/Al-DS) and its grafted with triethoxymethylsilane (TEMS), (TEMS-g-Mg/Al-DS) were synthesized through co-precipitation and salinization reaction methods. The presence of alkyl group, v(C-H) in both LDH had confirmed through Fourier transform infrared (FTIR). The appearance of peaks in FTIR spectra within the absorbance range of 2800 – 2930 cm-1indicates a successful surface modification of LDH, supported by the changes of interlayer spacing and the presence of carbon from X-ray diffractogram and CHNS elemental analysis, respectively. The synthesized LDH was mixed with LDPE via melt intercalation method. The LDH modification resulted in higher interaction and compatibility between the LDPE matrix and LDH by the formation exfoliated type of nanocomposites, as suggested by XRD analysis.
Mild steel plays an essential part in many construction industries due to its low cost and excellent mechanical properties. However, the use of strong acid in pickling, construction, and oil refining processes adds to a serious corrosion problem for mild steel. Two Cu(II) dithiocarbamate (DTC) complexes were successfully synthesised, namely Cu(II) ethyl-benzyl DTC (Cu[EtBenzdtc]2) and Cu(II) butyl-methyl DTC (Cu[BuMedtc]2) complexes, by a condensation reaction and subsequently used to scrutinise the corrosion resistance activity towards mild steel in acidic media. The proposed structures of complexes were characterised by using the Fourier transform infrared (FTIR) and ultraviolet-visible (UV-Vis) spectroscopies. The melting point for Cu[EtBenzdtc]2 was found around 362–375°C, and 389–392°C for Cu[BuMedtc]2. The percentages of Cu(II) found in Cu[EtBenzdtc]2 and Cu[BuMedtc]2 were 7.6% and 7.5%, respectively. Both complexes were non-electrolyte based on the molar conductivity analysis. Their corrosion inhibition performances were tested by using a weight loss measurement. Cu[BuMedtc]2 showed a good result as a corrosion inhibitor compared to Cu[EtBenzdtc]2. The complexes showed good effectiveness in sulfuric acid (H2SO4) compared to hydrochloric acid (HCl) solution. Furthermore, Cu[BuMedtc]2 showed a good result as a corrosion inhibitor compared to Cu[EtBenzdtc]2 with the highest percentage of corrosion inhibition recorded at 91.8%. Meanwhile, the highest percentage of corrosion inhibition shown by Cu[EtBenzdtc]2 was only 86.9%. The lowest corrosion rate shown for Cu[BuMedtc]2 was 8.1944×10-4 cm-1 h-1. Meanwhile, the Cu[EtBenzdtc]2 showed the lowest corrosion rate only at 1.3194×10-3 cm-1 h-1. This implies that Cu[BuMedtc]2 showed lower corrosion rate but higher inhibition efficiency compared to Cu[EtBenzdtc]2.
Complex systems require rigorous analysis using effective method, in order to handle and interpret their information. Spectrum produced from Fourier transform infrared (FTIR) instrument is an example of a complex system, due to their overlapped bands and interactions within the spectrum. Thus, chemometrics techniques are required to further analyze the data, in particular, chemometrics fuzzy autocatalytic set (c-FACS). The c-FACS is initially used to analyze the FTIR spectra of gelatins. However, in this study, the c-FACS is generalized and implemented for analysis of Coronavirus disease 2019 (Covid-19), particularly, the pandemic outbreak in Malaysia. The daily Covid-19 cases in states in Malaysia are modeled and analyzed using c-FACS, to observe the trend and severity of the disease in Malaysia. As a result, the classification of severity of zones in Malaysia are identified. The obtained results offer descriptive insight for strategizing purposes in combating the Covid-19 outbreak in Malaysia.
This study reports the caffeine content in seven locally available coffee. The caffeine was extracted with chloroform and analysed using Fourier Transform Infrared (FTIR). The method reports an average recovery of 101% with the limit of determination established at 0.1%. The absorption band at 1654 cm-1 was used to construct the calibration curve for quantification of caffeine where the regression was fitted with satisfactory linearity. An average of 0.55% of caffeine was detected in the seven coffee products with Arabica coffee demonstrating lower caffeine concentration. The study evidenced that caffeine content in coffee is determined by the coffee types. The caffeine content found in the local coffee products was relatively lower likely due to the solvent types, extraction procedure and analytical method used.