Baeckea frutescens or locally known as Cucur atap is used as antibacterial, antidysentery, antipyretic and diuretic agent. In Malaysia and Indonesia, they are used as an ingredient of the traditional medicine given to mothers during confinement. A three-steps infra-red (IR) macro-fingerprinting method combining conventional IR spectra, and the secondary derivative spectra with two dimensional infrared correlation spectroscopy (2D-IR) have been proved to be effective methods to examine a complicated mixture such as herbal medicines. This study investigated the feasibility of employing multi-steps IR spectroscopy in order to study the main constituents of B. frutescens and its different extracts (extracted by chloroform, ethyl acetate, methanol and aqueous in turn). The findings indicated that FT-IR and 2D-IR can provide many holistic variation rules of chemical constituents. The structural information of the samples indicated that B. frutescens and its extracts contain a large amount of flavonoids, since some characteristic absorption peaks of flavonoids, such as ∼1600cm(-1), ∼1500cm(-1), ∼1450cm(-1), and ∼1270cm(-1) can be observed. The macroscopical fingerprint characters of FT-IR and 2D-IR spectra can not only provide the information of main chemical constituents in medicinal materials and their different extracts, but also compare the components differences among the similar samples. In conclusion, the multi-steps IR macro-fingerprint method is rapid, effective, visual and accurate for pharmaceutical research.
Microencapsulation is a process by which tiny parcels of an active ingredient are packaged within a second material for the purpose of shielding the active ingredient from the surrounding environment. This study aims to determine the ability of the microencapsulation technique to improve the viability of Trichoderma harzianum UPM40 originally isolated from healthy groundnut roots as effective biological control agents (BCAs). Alginate was used as the carrier for controlled release, and montmorillonite clay (MMT) served as the filler. The encapsulated Ca-alginate-MMT beads were characterised using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The FTIR results showed the interaction between the functional groups of alginate and MMT in the Ca-alginate-MMT beads. Peaks at 1595, 1420 and 1020 cm(-1) characterised alginate, and peaks at 1028 and 453 cm(-1) characterised MMT; both sets of peaks appeared in the Ca-alginate-MMT FTIR spectrum. The TGA analysis showed an improvement in the thermal stability of the Ca-alginate-MMT beads compared with the alginate beads alone. SEM analysis revealed a homogeneous distribution of the MMT particles throughout the alginate matrix. T. harzianum UPM40 was successfully encapsulated in the Ca-alginate-MMT beads. Storage analysis of the encapsulated T. harzianum UPM40 showed that the low storage temperature of 5°C resulted in significantly (p
Plastic waste constitutes the third largest waste volume in Malaysian municipal solid waste (MSW), next to putrescible waste and paper. The plastic component in MSW from Kuala Lumpur averages 24% (by weight), whereas the national mean is about 15%. The 144 waste dumps in the country receive about 95% of the MSW, including plastic waste. The useful life of the landfills is fast diminishing as the plastic waste stays un-degraded for more than 50 years. In this study the compostability of polyethylene and pro-oxidant additive-based environmentally degradable plastics (EDP) was investigated. Linear low-density polyethylene (LLDPE) samples exposed hydrolytically or oxidatively at 60 degrees C showed that the abiotic degradation path was oxidative rather than hydrolytic. There was a weight loss of 8% and the plastic has been oxidized as shown by the additional carbonyl group exhibited in the Fourier transform infra red (FTIR) Spectrum. Oxidation rate seemed to be influenced by the amount of pro-oxidant additive, the chemical structure and morphology of the plastic samples, and the surface area. Composting studies during a 45-day experiment showed that the percentage elongation (reduction) was 20% for McD samples [high-density polyethylene, (HDPE) with 3% additive] and LL samples (LLDPE with 7% additive) and 18% reduction for totally degradable plastic (TDP) samples (HDPE with 3% additive). Lastly, microbial experiments using Pseudomonas aeroginosa on carbon-free media with degradable plastic samples as the sole carbon source, showed confirmatory results. A positive bacterial growth and a weight loss of 2.2% for degraded polyethylene samples were evident to show that the degradable plastic is biodegradable.
The identification, characterization and quantification of crystal forms are becoming increasingly important within the pharmaceutical industry. A combination of different physical analytical techniques is usually necessary for this task. In this work solid-state techniques, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and X-ray powder diffractometry (XRPD) were combined to analyze polymorphic purity of crystalline ranitidine-HCl, an antiulcer drug, H2 receptor antagonists. A series of 12 different mixtures of Form 1 and 2 was prepared by geometric mixing and their DRIFT spectra and XRD powder patterns were obtained and analyzed, either alone or combined together, using Artificial Neural Networks (ANNs). A standard feed-forward network, with back-propagation rule and with multi layer perceptron architecture (MPL) was chosen. A working range of 1.0-100% (w/w) of crystal Form 2 in Form 1 was established with a minimum quantifiable level (MQL) of 5.2% and limit of detection of 1.5% (w/w). The results demonstrate that DRIFTS combined with XRPD may be successfully used to distinguish between the ranitidine-HCl polymorphs and to quantify the composition of binary mixtures of the two.
Treated Rhizopora mucronata tannin (RMT) as a corrosion inhibitor for carbon steel and copper in oil and gas facilities was investigated. Corrosion rate of carbon-steel and copper in 3wt% NaCl solution by RMT was studied using chemical (weight loss method) and spectroscopic (FTIR) techniques at various temperatures in the ranges of 26-90°C. The weight loss data was compared to the electrochemical by the application of Faraday's law for the conversion of corrosion rate data from one system to another. The inhibitive efficiency of RMT was compared with commercial inhibitor sodium benzotriazole (BTA-S). The best concentration of RMT was 20% (w/v), increase in concentration of RMT decreased the corrosion rate and increased the inhibitive efficiency. Increase in temperature increased the corrosion rate and decreased the inhibitive efficiency but, the rate of corrosion was mild with RMT. The FTIR result shows the presence of hydroxyl group, aromatic group, esters and the substituted benzene group indicating the purity of the tannin. The trend of RMT was similar to that of BTA-S, but its inhibitive efficiency for carbon-steel was poor (6%) compared to RMT (59%). BTA-S was efficient for copper (76%) compared to RMT (74%) at 40% (w/v) and 20% (w/v) concentration respectively. RMT was efficient even at low concentration therefore, the use of RMT as a cost effective and environmentally friendly corrosion inhibiting agent for carbon steel and copper is herein proposed.
Fenton oxidation, an advanced oxidation process, is an efficient method for the treatment of recalcitrant wastewaters. Unfortunately, it utilizes H2O2 and iron-based homogeneous catalysts, which lead to the formation of high volumes of sludge and secondary pollutants. To overcome these problems, an alternate option is the usage of heterogeneous catalyst. In this study, a heterogeneous catalyst was developed to provide an alternative solution for homogeneous Fenton oxidation. Iron Zeolite Socony Mobile-5 (Fe-ZSM-5) was synthesized using a new two-step process. Next, the catalyst was characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, fourier transform infrared spectroscopy, and Brunauer-Emmett-Teller analysis and tested against a model wastewater containing the azo dye Acid Blue 113. Results showed that the loading of iron particles reduced the surface area of the catalyst from 293.59 to 243.93 m2/g; meanwhile, the average particle size of the loaded material was 12.29 nm. Furthermore, efficiency of the developed catalyst was evaluated by performing heterogeneous Fenton oxidation. Taguchi method was coupled with principal component analysis in order to assess and optimize mineralization efficiency. Experimental results showed that under optimized conditions, over 99.7% degradation and 77% mineralization was obtained, with a 90% reduction in the consumption of the developed catalyst. Furthermore, the developed catalyst was stable and reusable, with less than 2% leaching observed under optimized conditions. Thus, the present study proved that newly developed catalyst has enhanced the oxidation process and reduced the chemicals consumption.
Polyimide/SiO(2) composite films were prepared from tetraethoxysilane (TEOS) and poly(amic acid) (PAA) based on aromatic diamine (4-aminophenyl sulfone) (4-APS) and aromatic dianhydride (3,3,4,4-benzophenonetetracarboxylic dianhydride) (BTDA) via a sol-gel process in N-methyl-2-pyrrolidinone (NMP). The prepared polyimide/SiO(2) composite films were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and thermogravimetric analysis (TGA). The FTIR results confirmed the synthesis of polyimide (4-APS/BTDA) and the formation of SiO(2) particles in the polyimide matrix. Meanwhile, the SEM images showed that the SiO(2) particles were well dispersed in the polyimide matrix. Thermal stability and kinetic parameters of the degradation processes for the prepared polyimide/SiO(2) composite films were investigated using TGA in N(2) atmosphere. The activation energy of the solid-state process was calculated using Flynn-Wall-Ozawa's method without the knowledge of the reaction mechanism. The results indicated that thermal stability and the values of the calculated activation energies increased with the increase of the TEOS loading and the activation energy also varied with the percentage of weight loss for all compositions.
In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.
Oxidation of sulfide in aqueous solution by hydrogen peroxide was investigated in the presence of hydrated ferric oxide catalyst. The ferric oxide catalyst was synthesized by sol gel technique from ferric chloride and ammonia. The synthesized catalyst was characterized by Fourier transform infrared spectroscopy, X-Ray diffraction analysis, scanning electrom microscope and energy dispersive X-ray analysis. The catalyst was quite effective in oxidizing the sulfide by hydrogen peroxide. The effects of sulfide concentration, catalyst loading, H2O2 dosing and temperature on the kinetics of sulfide oxidation were investigated. Kinetic equations and activation energies for the catalytic oxidation reaction were calculated based on the experimental results.
This paper reports the synthesis, characterization, anticancer screening and quantum chemical calculation of a tetradentate Schiff base 2,2'-((1E,1'E)-((2,2-dimethylpropane-1,3-diyl)bis- (azanylylidene))bis(methanylylidene))bis(4-fluorophenol) (L2F) and its Pd (II) complex (PdL2F). The compounds were characterized via UV-Visible, NMR, IR spectroscopy and single crystal x-ray diffraction. Density Functional Theory (DFT) and time-dependent DFT calculations in gas and solvent phases were carried out using B3LYP, B3P86, CAM-B3LYP and PBE0 hybrid functionals combined with LanL2DZ basis set. Complexation of L2F to form PdL2F was observed to cause a bathochromic shift of the maximum absorption bands of n-π* from 327 to 410 nm; an upfield shift for δ (HC = N) from 8.30 to 7.96 ppm and a decreased wavenumber for ν(C = N) from 1637 to 1616 cm-1. Overall, the UV-Vis, NMR and IR spectral data are relatively well reproduced through DFT and TD-DFT methods. L2F and PdL2F showed IC50 of 90.00 and 4.10 μg/mL, respectively, against human colorectal carcinoma (HCT116) cell lines, signifying increased anticancer activity upon complexation with Pd (II).
The present work describes the successful functionalization/magnetization of bio-polymeric spores of Lycopodium clavatum (sporopollenin) with 1-(2-hydroxyethyl) piperazine. Analytical techniques, i.e., Fourier transform infrared (FT-IR), field emission scanning electron microscope (FESEM), energy-dispersive X-ray spectroscopy (EDS), and vibrating sample magnetometer (VSM), were used to confirm the formation of 1-(2-hydroxyethyl) piperazine-functionalized magnetic sporopollenin (MNPs-Sp-HEP). The proposed adsorbent (MNPs-Sp-HEP) was used for the removal of noxious Pb(II) and As(III) metal ions from aqueous media through a batch-wise method. Different experimental parameters were optimized for the effective removal of selected noxious metal ions. Maximum adsorption capacity (q m ) 13.36 and 69.85 mg g-1 for Pb(II) and As(III), respectively, were obtained. Thermodynamic parameters such as free energy (ΔG°), entropy (ΔS°), and enthalpy (ΔH°) were also studied from the adsorption results and were used to elaborate the mechanism of their confiscation. The obtained results indicated that newly adsorbent can be successfully applied for the decontamination of noxious Pb(II) and As(III) from the aqueous environment.
The current study aimed to investigate the efficiencies and mechanisms of slag filter media for removing phosphorus from synthetic wastewater. The steel slag with high ferric oxides (Fe2O3) was subjected for the electric arc furnace (EAF) and selected as the filter media (HFe). The chemical characteristics of HFe were determined using pH, point of zero charge (PZC) and XRF. The phosphorus removal efficiency was studied in a designed vertical steel slag column rock filters in unaerated HFe (UEF) and aerated HFe (AEF) system. The microstructure of HFe was analyzed by FTIR, XRD and SEM-EDX analysis. The results of XRF revealed that ferric oxide (Fe2O3) ranged from 26.1 to 38.2%. PZC for Filter HFe was recorded at pH 10.55 ± 0.27. The highest efficiencies were recorded by UEF and AEF systems at pH 3 and pH 5 (89.97 ± 4.02% and 79.95 ± 6.25% at pH 3 and 72.97 ± 8.38% and 66.00 ± 12.85% at pH 5 for UEF and AEF, respectively). These findings indicated that AEF exhibiting higher removal than UEF systems might be due to presence high Fe concentration in AEF which play important role in the phosphorus removal. The main elements available on the surface of HFe included carbon, oxygen, iron, calcium, magnesium, silicon, platinum, sulphur, manganese, titanium and aluminium. The XRD analysis indicated that the precipitation of orthophosphate as calcium and iron-phosphates was the removal mechanism as confirmed using FT-IR analysis. These findings demonstrated the efficiency of HFe in removing of phosphorus from wastewater.
In this study, the effects of lignin modification on the properties of kenaf core fiber reinforced poly(butylene succinate) biocomposites were examined. A weight percent gain (WPG) value of 30.21% was recorded after the lignin were modified with maleic anhydride. Lower mechanical properties were observed for lignin composites because of incompatible bonding between the hydrophobic matrix and the hydrophilic lignin. Modified lignin (ML) was found to have a better interfacial bonding, since maleic anhydrides remove most of the hydrophilic hydrogen bonding (this was proven by a Fourier-transform infrared (FTIR) spectrometer-a reduction of broadband near 3400 cm-1, corresponding to the -OH stretching vibration of hydroxyl groups for the ML samples). On the other hand, ML was found to have a slightly lower glass transition temperature, Tg, since reactions with maleic anhydride destroy most of the intra- and inter-molecular hydrogen bonds, resulting in a softer structure at elevated temperatures. The addition of kraft lignin was found to increase the thermal stability of the PBS polymer composites, while modified kraft lignin showed higher thermal stability than pure kraft lignin and possessed delayed onset thermal degradation temperature.
Actinidin was used to pretreat the bovine hide and ultrasonic wave (53 kHz and 500 W) was used for the time durations of 2, 4 and 6 h at 60 °C to extract gelatin samples (UA2, UA4 and UA6, respectively). Control (UAC) gelatin was extracted using ultrasound for 6 h at 60 °C without enzyme pretreatment. There was significant (p < 0.05) increase in gelatin yield as the time duration of ultrasound treatment increased with UA6 giving the highest yield of 19.65%. Gel strength and viscosity of UAC and UA6 extracted gelatin samples were 627.53 and 502.16 g and 16.33 and 15.60 mPa.s, respectively. Longer duration of ultrasound treatment increased amino acids content of the extracted gelatin and UAC exhibited the highest content of amino acids. Progressive degradation of polypeptide chains was observed in the protein pattern of the extracted gelatin as the time duration of ultrasound extraction increased. Fourier transform infrared (FTIR) spectroscopy depicted loss of molecular order and degradation in UA6. Scanning electron microscopy (SEM) revealed protein aggregation and network formation in the gelatin samples with increasing time of ultrasound treatment. The study indicated that ultrasound assisted gelatin extraction using actinidin exhibited high yield with good quality gelatin.
Polymer composites are favorite materials for sensing applications due to their low cost and easy fabrication. In the current study, composite nanofibers consisting of polyethylene oxide (PEO), oxidized multi-walled carbon nanotubes (MWCNT) and copper oxide (CuO) nanoparticles with 1% and 3% of fillers (i.e., PEO-CuO-MWCNT: 1%, and PEO-CuO-MWCNT: 3%) were successfully developed through electrospinning for humidity sensing applications. The composite nanofibers were characterized by FTIR, XRD, SEM and EDX analysis. Firstly, they were loaded on an interdigitated electrode (IDE), and then the humidity sensing efficiency was investigated through a digital LCR meter (E4980) at different frequencies (100 Hz-1 MHz), as well as the percentage of relative humidity (RH). The results indicated that the composite nanofibers containing 1% and 3% MWCNT, combined with CuO in PEO polymer matrix, showed potent resistive and capacitive response along with high sensitivity to humidity at room temperature in an RH range of 30-90%. More specifically, the PEO-CuO-MWCNT: 1% nanocomposite displayed a resistive rapid response time within 3 s and a long recovery time of 22 s, while the PEO-CuO-MWCNT: 3% one exhibited 20 s and 11 s between the same RH range, respectively.
In this work, hydrogels were prepared from carboxymethyl cellulose (CMC) and 1-vinyl-2-pyrrolidone(VP) by Electron Beam irradiation in the presence of N,N'-methylenebisacrylamide (BIS) as a crosslinkingagent. The parameters studied include stirring time and percentage of crosslinking agent. Hydrogels werecharacterized using Fourier Transform Infrared (FTIR) spectroscopy and Scanning Electron Microscopy(SEM). VP and BIS were found be effective as reinforcement materials to improve the properties ofCMC. Meanwhile, the optimum conditions were 5% BIS and 3 hours of stirring time. The gel fractionincreased when irradiation dose was increased. FTIR confirmed the crosslinking reaction between CMCand VP after the irradiation process by using BIS as the crosslinking agent. TGA thermograms showedchanges in the thermal properties of CMC-VP hydrogels in the presence of different amounts of BIS.
Polyaniline (PANI) and polyaniline composites with aluminium oxide (Al2O3) were prepared using the in situ polymerization method. The composites were then blended with acrylic paint and applied to carbon steel panels. The coated steel panels were evaluated for corrosion using the immersion test technique. The results revealed that the steel panels coated with polyaniline composites and with Al2O3 containing coatings had small corrosion as compared to the bare sample and the samples coated with polyaniline and paint alone. The samples were characterized by Fourier transform infrared (FTIR) and X-ray diffraction(XRD). In addition, the morphology of the finished samples was observed using the scanning electron microscopy (SEM). This novel composite was used as a paint pigment for enhancing the barrier properties and the paint protectable against aggressive ions. Meanwhile, corrosion was evaluated through visual monitoring using a digital camera after 60 days of fully immersion test in 5% NaCl. The weight loss method was also used to evaluate corrosion.
Boron has been classified as a drinking water pollutant in many countries. It is harmful to many plants, exceptionally sensible plants, and human health. Therefore, boron level needs to be decreased to 0.3 mg/L for drinking water and within 0.5 mg/L to 1 mg/L for irrigation water. In this study, various operational parameters namely pH, contact time and liquid/solid ratio were investigated to determine the potential of using date seed (or date pit or date stone) to remove boron from seawater. This study's main objective was to determine boron adsorption capacities of date seeds prepared by various methods (i.e., powdered, activated, acid-treated and defatted seed) by batch adsorption process using boron contaminated synthetic seawater. The process parameters of the selected biosorbent among the four date seed preparations methods were optimized. The surface characteristics were analyzed by using Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscope (SEM). The results showed that acid-treated date seed was the best biosorbent in terms of removing 89.18% boron from aqueous solution at neutral pH, liquid to solid ratio of 5 within 2 hours of reaction time at room temperature (25°C±2°C).
Epoxidized natural rubber/polyvinyl chloride/microcrystalline cellulose (ENR/PVC/MCC) composite membranes were
prepared and used to treat palm oil mill effluent (POME). The loadings of MCC were varied at 0, 5, 10 and 15 w/w%. The
increment of MCC loads has intensified the hydroxyl peak of the membranes in FTIR spectrum, indicating the increase
in membrane hydrophilicity. MCC acted as a pore forming agent since the ENR/PVC/10% MCC gave the highest water
flux and well-distributed pores. After first treatment of POME, the levels of chemical oxygen demand (COD), biochemical
oxygen demand (BOD) and total suspended solid (TSS) were reduced to 99.9%, 70.3%, and 16.9%, respectively. These
data showed that ENR/PVC/MCC membrane has the potential to treat POME.
α-Mangostin is an oxygenated heterocyclic xanthone with remarkable pharmacological properties, but poor aqueous solubility and low oral bioavailability hinder its therapeutic application. This study sought to improve the compound's solubility and study the mechanism underlying solubility enhancement. Solid dispersions of α-mangostin were prepared in polyvinylpyrrolidone (PVP) by solvent evaporation method and showed substantial enhancement of α-mangostin's solubility from 0.2 ± 0.2 μg/mL to 2743 ± 11 μg/mL. Fourier transform infrared spectroscopy and differential scanning calorimetry indicated interaction between α-mangostin and PVP. Transmission electron microscopy and dynamic light scattering showed self-assembly of round anionic nanomicelles with particle size in the range 99-127 nm. Powder X-ray diffraction indicated conversion of α-mangostin from crystalline into amorphous state, and scanning electron microscopy showed the presence of highly porous powder. Studies using the fluorescent probe pyrene showed that the critical micellar concentration is about 77.4 ± 4 μg/mL. Cellular uptake of nanomicelles was found to be mediated via endocytosis and indicated intracellular delivery of α-mangostin associated with potent cytotoxicity (median inhibitory concentration of 8.9 ± 0.2 μg/mL). Improved solubility, self-assembly of nanomicelles, and intracellular delivery through endocytosis may enhance the pharmacological properties of α-mangostin, particularly antitumor efficacy.