The analytical methods for the determination of the amine solvent properties do not provide input data for real-time process control and optimization and are labor-intensive, time-consuming, and impractical for studies of dynamic changes in a process. In this study, the potential of nondestructive determination of amine concentration, CO2 loading, and water content in CO2 absorption solvent in the gas processing unit was investigated through Fourier transform near-infrared (FT-NIR) spectroscopy that has the ability to readily carry out multicomponent analysis in association with multivariate analysis methods. The FT-NIR spectra for the solvent were captured and interpreted by using suitable spectra wavenumber regions through multivariate statistical techniques such as partial least square (PLS). The calibration model developed for amine determination had the highest coefficient of determination (R2) of 0.9955 and RMSECV of 0.75%. CO2 calibration model achieved R2 of 0.9902 with RMSECV of 0.25% whereas the water calibration model had R2 of 0.9915 with RMSECV of 1.02%. The statistical evaluation of the validation samples also confirmed that the difference between the actual value and the predicted value from the calibration model was not significantly different and acceptable. Therefore, the amine, CO2, and water models have given a satisfactory result for the concentration determination using the FT-NIR technique. The results of this study indicated that FT-NIR spectroscopy with chemometrics and multivariate technique can be used for the CO2 solvent monitoring to replace the time-consuming and labor-intensive conventional methods.
Poly(phenyl-(4-(6-thiophen-3-yl-hexyloxy)-benzylidene)-amine) (P3TArH) was successfully synthesized and coated on the surface of Fe₃O₄ magnetic nanoparticles (MNPs). The nanocomposites were characterized by Fourier transform infra-red (FTIR), X-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) surface area analysis, analyzer transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). P3TArH-coated MNPs (MNP@P3TArH) showed higher capabilities for the extraction of commonly-used phthalates and were optimized for the magnetic-solid phase extraction (MSPE) of environmental samples. Separation and determination of the extracted phthalates, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dicyclohexyl phthalate (DCP), di-ethylhexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP), were conducted by a gas chromatography-flame ionization detector (GC-FID). The best working conditions were as follows; sample at pH 7, 30 min extraction time, ethyl acetate as the elution solvent, 500-µL elution solvent volumes, 10 min desorption time, 10-mg adsorbent dosage, 20-mL sample loading volume and 15 g·L-1 concentration of NaCl. Under the optimized conditions, the analytical performances were determined with a linear range of 0.1⁻50 µg·L-1 and a limit of detection at 0.08⁻0.468 µg·L-1 for all of the analytes studied. The intra-day (n = 7) and inter-day (n = 3) relative standard deviations (RSD%) of three replicates were each demonstrated in the range of 3.7⁻4.9 and 3.0⁻5.0, respectively. The steadiness and reusability studies suggested that the MNP@P3TArH could be used up to five cycles. The proposed method was executed for the analysis of real water samples, namely commercial bottled mineral water and bottled fresh milk, whereby recoveries in the range of 68%⁻101% and RSD% lower than 7.7 were attained.
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.
Four strains of bioflocculant-producing bacteria were isolated from a palm oil mill effluent (POME). The four bacterial strains were identified as Pseudomonas alcaliphila (B1), Pseudomonas oleovorans (B2), Pseudomonas chengduensis (B3), and Bacillus nitratireducens (B4) by molecular identification. Among the four bacterial strains, Bacillus nitratireducens (B4) achieved the highest flocculating activity (49.15%) towards kaolin clay suspension after eight hours of cultivation time and was selected for further studies. The optimum conditions for Eriochrome Black T (EBT) flocculation regarding initial pH, type of cation, and B4 dosage were determined to be pH 2, Ca2⁺ cations, and a dosage of 250 mL/L of nutrient broth containing B4. Under these conditions, above 90% of EBT dye removal was attained. Fourier transform infrared spectroscopic (FT-IR) analysis of the bioflocculant revealed the presence of hydroxyl, alkyl, carboxyl, and amino groups. This bioflocculant was demonstrated to possess a good flocculating activity, being a promissory, low-cost, harmless, and environmentally friendly alternative for the treatment of effluents contaminated with dyes.
Polychloropolymethylstyrene (PCMS) polymers were synthesized with clay Cloisite and without clay Cloisite and chloromethylstyrene (CMS) combine with styrene (1:1) v/v or known as copolymer and clay Cloisite by the polymerization process. The attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectra of each polymer synthesized are reported. The spectra of IR shows the different value of the wavenumber and intensity for each set of different sample. The spectra can be as a reference for others to use in synthesizing this polymer and clay Cloisite for different type of application.
Biomass from oil palm frond leaves (OPFL) is an excellent reservoir of lignocellulosic material which full potential remains untapped. This study aimed to statistically optimize the covalent immobilization of Candida rugosa lipase (CRL) onto a ternary support comprised of OPFL derived nanocellulose (NC) and montmorillonite (MMT) in alginate (ALG) (CRL-ALG/NC/MMT). The coarser topology and the presence of characteristic spherical globules in the field emission scanning electron micrographs and atomic force micrographs, respectively, supported the existence of CRL on ALG/NC/MMT. In addition, amide peaks at 3478 and 1640 cm-1 in the fourier transform infrared spectra affirmed that CRL was covalently bonded to ALG/NC/MMT. The optimized Taguchi Design-assisted immobilization of CRL onto ALG/NC/MMT (7 h of immobilization, 35℃, pH 5, 7 mg/mL protein loading) gave a production yield of 92.89 % of ethyl levulinate (EL), as proven by gas chromatography-mass spectrometric ([M] +m/z 144, C7H12O3), FTIR and nuclear magnetic resonance (CAS-539-88-8) data. A higher optimal reaction temperature (50℃) and the reusability of CRL-ALG/NC/MMT for up to 9 esterification cycles substantiated the appreciable structural rigidification of the biocatalyst by ALG/NC/MMT, which improved the catalytic activity and thermal stability of the lipase.
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
This study demonstrated the utilization of radiation-induced initiator methods for the formation of
nanoparticles of Acrylated Palm Oil (APO) using aqueous Pluronic F-127 (PF-127) microemulsion
system. This microemulsion system was subjected to gamma irradiation to form the crosslinked APO
nanoparticles. Dynamic light scattering (DLS), Fourier Transform Infrared (FTIR) spectroscopy and
Transmission Electron Microscopy (TEM) were used to characterize the size and the chemical structure
of the nanoparticles. As a result, the size of the APO nanoparticle was decreased when the irradiation
dose increased. The decrease in size might be due to the effects of intermolecular crosslinking and
intramolecular crosslinking reactions of the APO nanoparticles during irradiation process. The size of the
nanoparticle is in the range of 98 to 200 nanometer (nm) after irradiation using gamma irradiator. This radiation-induced method provides a free initiator
induced and easy to control process as compared
to the classical or chemical initiator process. The
study has shown that radiation-induced initiator
methods, namely, polymerization and crosslinking
in the microemulsion, were promising for the
synthesis of nanoparticles.
The use of Fourier transform infrared (FTIR) spectroscopy coupled with chemometric techniques to differentiate butter from beef fat (BF) was investigated. The spectral bands associated with butter, BF, and their mixtures were scanned, interpreted, and identified by relating them to those spectroscopically representative to pure butter and BF. For quantitative analysis, partial least square (PLS) regression was used to develop a calibration model at the selected fingerprint regions of 1500-1000 cm-1, with the values of coefficient of determination (R2) and root mean square error of calibration (RMSEC) are 0.999 and 0.89% (v/v), respectively. The PLS calibration model was subsequently used for the prediction of independent samples containing butter in the binary mixtures with BF. Using 6 principal components, root mean square error of prediction (RMSEP) is 2.42% (v/v). These results proved that FTIR spectroscopy in combination with multivariate calibration can be used for the detection and quantification of BF in butter formulation for authentication use.
The coordination complexes of Co(II) and Zn(II) with Schiff bases derived from ophenylenediamine and substituted 2-hydroxybenzaldehyde were prepared. All compounds were characterized by Fourier transform infrared (FTIR) spectroscopy and Nuclear magnetic resonance (NMR) spectroscopy elemental analyzers. They were analyzed using impedance spectroscopy in the frequency range of 100Hz - 1MHz. L1 and L2 showed higher conductivity compared to their metal
complexes, which had values of 1.37 x 10-7 and 6.13 x 10-8S/cm respectively.
Combined multiple 2D views (proximal, anterior and ventral aspects) of the sagittal otolith are proposed here as a method to capture shape information for fish classification. Classification performance of single view compared with combined 2D views show improved classification accuracy of the latter, for nine species of Sciaenidae. The effects of shape description methods (shape indices, Procrustes analysis and elliptical Fourier analysis) on classification performance were evaluated. Procrustes analysis and elliptical Fourier analysis perform better than shape indices when single view is considered, but all perform equally well with combined views. A generic content-based image retrieval (CBIR) system that ranks dissimilarity (Procrustes distance) of otolith images was built to search query images without the need for detailed information of side (left or right), aspect (proximal or distal) and direction (positive or negative) of the otolith. Methods for the development of this automated classification system are discussed.
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.
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 paper outlines the application of chemometrics and pattern recognition tools to classify palm oil using Fourier Transform Mid Infrared spectroscopy (FT-MIR). FT-MIR spectroscopy is used as an effective analytical tool in order to categorise the oil into the category of unused palm oil and used palm oil for frying. The samples used in this study consist of 28 types of pure palm oil, and 28 types of frying palm oils. FT-MIR spectral was obtained in absorbance mode at the spectral range from 650 cm -1 to 4000 cm -1 using FT-MIR-ATR sample handling. The aim of this work is to develop fast method in discriminating the palm oils by implementing Partial Least Square Discriminant Analysis (PLS-DA), Learning Vector Quantisation (LVQ) and Support Vector Machine (SVM). Raw FT-MIR spectra were subjected to Savitzky-Golay smoothing and standardized before developing the classification models. The classification model was validated through finding the value of percentage correctly classified by test set for every model in order to show which classifier provided the best classification. In order to improve the performance of the classification model, variable selection method known as t-statistic method was applied. The significant variable in developing classification model was selected through this method. The result revealed that PLSDA classifier of the standardized data with application of t-statistic showed the best performance with highest percentage correctly classified among the classifiers.
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.
Neat cellulose acetate (CA) and CA/polysulfone (PSf) blend ultrafiltration membranes in the presence of polyvinylpyrrolidone as a pore former were prepared via a phase inversion technique. The prepared membranes were characterized by Fourier transform infrared, scanning electron microscopy, mechanical strength, water content, porosity, permeate flux and heavy metals (Pb2+, Cd2+, Zn2+ and Ni2+) rejection to comprehend the impact of polymer blend composition and additive on the properties of the modified membranes. The water flux expanded by increasing of PSf content in the polymer composition. CA/PSf (60/40) had the highest flux among prepared membranes. Prepared blend membranes were able to remove heavy metals from water in the following order: Pb2+ > Cd2+ > Zn2+ > Ni2+. The CA/PSf (80/20) blend membrane had great performance among prepared membranes due to the high heavy metals removal and permeate flux.
New compound, namely (Z)-1-[4-(trifluoromethyl)benzylidene]thiosemicarbazide was successfully synthesized using thiosemicarbazide with 4-(trifluoromethyl)-benzaldehyde in ethanol solution. The data presented in this articles is related to our research articles entitled "Crystal Structure of (Z)-1-[4-(Trifluoromethyl)benzylidene]thiosemicarbazide" (Osman et al., 2017) [1]. This work shows the continue data from experimental spectroscopic measurement which are Fourier Transform Infrared (FTIR) and 13C Nuclear Magnetic Resonance (13C NMR). Assessment on the correlation with theoretical computational data was also carried out through GaussView 5.0.9 and Gaussian09 software. Molecular Electrostatic Potential (MEP) and Highest Occupied Molecular Orbital-Lowest Unoccupied Molecular Orbital (HOMO-LUMO) were also illustrated.
In this work, epoxidized natural rubber 50 (ENR-50) has been used as a host polymer for the preparation of electrolyte system. Attenuated total reflection-fourier transform infrared spectroscopic analyses showed the presence of lithium saltENR interactions. The glass transition temperature displayed an increasing trend with the increase in salt concentration indicating that the ionic conductivity was not influenced by segmental motion of the ENR-50 chains. The increase in
glass transition temperature with the addition of salt was due to the formation of transient cross-linking between ENR-50 chains via the coordinated interaction between ENR-50 chains and salt. The highest room temperature ionic conductivity obtained was in the order of 10-5 S cm-1 for the film containing 50 wt% of lithium salt. The ionic conductivity of this electrolyte system increased with increasing temperature and obeyed the Vogel-Tamman-Fulcher behavior. The increase in ionic conductivity of the electrolyte system with salt concentration could also be correlated to the charge carriers concentration and/or migration rate of charge carriers.
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.