This present study investigated the effect of Captisol, a chemically modified cyclodextrin, on the in vitro dissolution of glimepiride. We prepared glimepiride-Captisol complexes of different mass ratios (1:1, 1:2, and 1:3 w/w) by a physical mixing or freeze-drying technique, and found that complexation with Captisol enhanced the water solubility of glimepiride. Molecular docking and dynamic simulation predicted complex formation; at the same time, Fourier transform infrared spectroscopy, differential scanning calorimetry, powder X-ray diffractometry, and scanning electron microscope indicated molecular interactions that support complexation. We also found that an inclusion complex was better than a physical mixture in enhancing the complexation of glimepiride with Captisol and enhancing water solubility. Phase solubility study of the glimepiride-Captisol complex showed an AL-type profile, implying the formation of a 1:1 inclusion complex. The study also revealed that pH influenced the stability of the complex because the stability constant of the glimepiride-Captisol complex was higher in distilled water of pH ∼6.0 than in phosphate buffer of pH 7.2.
In the present work, a novel polymer composite electrolytes (PCEs) based on poly(vinyl alcohol) (PVA): ammonium thiocyanate (NH4SCN): Cd(II)-complex plasticized with glycerol (Gly) are prepared by solution cast technique. The film structure was examined by XRD and FTIR routes. The utmost ambient temperature DC ionic conductivity (σDC) of 2.01 × 10-3 S cm-1 is achieved. The film morphology was studied by field emission scanning electron microscopy (FESEM). The trend of σDC is further confirmed with investigation of dielectric properties. Transference numbers of ions (tion) and electrons (tel) are specified to be 0.96 and 0.04, respectively. Linear sweep voltammetry (LSV) displayed that the PCE potential window is 2.1 V. The desired mixture of activated carbon (AC) and carbon black was used to fabricate the electrodes of the EDLC. Cyclic voltammetry (CV) was carried out by sandwiching the PCEs between two carbon-based electrodes, and it revealed an almost rectangular shape. The EDLC exhibited specific capacitance, energy density, and equivalent series resistance with average of 160.07F/g, 18.01Wh/kg, and 51.05Ω, respectively, within 450 cycles. The EDLC demonstrated the initial power density as 4.065 × 103 W/Kg.
In this research, an attempt to develop zwitterion composite adsorbent is conducted by modifying chitosan (CHS) with a covalent cross-linker (epichlorohydrin, ECH) and an aluminosilicate mineral (zeolite, ZL). The zwitterion composite adsorbent of chitosan-epichlorohydrin/zeolite (CHS-ECH/ZL) is performed multifunctional tasks by removing two structurally different cationic (methylene blue dye, MB), and anionic (reactive red 120 dye, RR120) dyes from aqueous solutions. The surface property, crystallinity, morphology, functionality, and charge of the CHS-ECH/ZL are analyzed using BET, XRD, SEM, FTIR, and pHpzc, analyses, respectively. The influence of pertinent parameters namely CHS-ECH/ZL dosage (0.02-0.5 g), solution pH (4-10), temperature (303-323K), initial dye concentration (30-400 mg/L), and contact time (0-600 min) on the MB and RR120 removal are tested. The research findings revealed that the adsorption isotherm at equilibrium well explained in according to the Freundlich isotherm model, and the recorded adsorption capacities of CHS-ECH/ZL are 156.1 and 284.2 mg/g for MB and RR120 respectively at 30 °C. The mechanism of MB and RR120 adsorption onto the CHS-ECH/ZL indicates various types of interactions namely, electrostatic interaction, hydrogen bonding, and Yoshida H-bonding in addition to n-π interaction. Overall, this research introduces CHS-ECH/ZL composite as an eco-friendly zwitterion adsorbent with good applicability towards the two structurally different cationic and anionic dyes from aqueous environment.
Titanium dioxide (TiO2) is added in sunscreens due to its ability to absorb ultraviolet (UV) light. However, upon irradiation of UV light, reactive oxygen species particularly hydroxyl radical which can damage human skin will be generated. In this study, lignin/TiO2 composites were employed to quench the hydroxyl radicals generated by the TiO2. The lignin was extracted from oil palm empty fruit bunch (OPEFB) via kraft and soda pulping processes. The kraft lignin composite was labelled as KL/TiO2 whereas the soda lignin composite was labelled as SL/TiO2. The lignins and the composites were characterized by FTIR, UV spectroscopy, 13C NMR, SEM, EDX, and XRD. The relative hydroxyl radical production of composites and TiO2 were compared through photo-oxidation of coumarin to 7-hydroxycoumarin as a test medium. The effect of types and amounts of lignin used were studied. The KL/TiO2 composite showed the least radical production due to higher phenolic hydroxyl content of kraft lignin. The activity of the hydroxyl radicals will be quenched when it abstract hydrogen atoms from the phenolic hydroxyl groups.
Two series of new hexasubstituted cyclotriphosphazene derivatives were successfully synthesized and characterized. These derivatives are differentiated by two types of linking units in the molecules such as amide-azo (6a-j) and azo-azo (8a-j). The homologues of the same series contain different terminal substituents such as heptyl, nonyl, decyl, dodecyl, tetradecyl, hydroxyl, carboxyl, chloro, nitro, and amino groups. All the intermediates and final compounds were characterized using Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), and Carbon, Hydrogen, and Nitrogen (CHN) elemental analysis. Liquid crystal properties for all compounds were determined using polarized optical microscope (POM). It was found that only intermediates 2a-e with nitro and alkoxyl terminal chains showed a smectic A phase. All the final compounds with alkoxyl substituents are mesogenic with either smectic A or C phases. However, other intermediates and compounds were found to be non-mesogenic. The study on the fire retardancy of final compounds was determined using limiting oxygen index (LOI) method. The LOI value of pure polyester resin (22.53%) was increased up to 24.71% after treating with 1 wt% of hexachlorocyclotriphosphazene (HCCP). Moreover, all the compounds gave positive results on the LOI values and compound 6i with the nitro terminal substituent showed the highest LOI value of 27.54%.
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.
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).
To overcome drawbacks in the conventional chemical route to synthesize eugenyl benzoate, immobilized Rhizomucor miehei lipase (RML) as the biocatalyst was proposed. The RML conjugated to a hybrid support consisting of biopolymers, chitosan (CS) and chitin nanowhiskers (CNWs). 1-ethyl-3-[3-dimethylaminopropyl]carbodiimide hydrochloride (EDAC) was used as the crosslinker to bind the lipase. Immobilization of RML was the highest on crosslinked CS/CNWs which gave a protein loading of ∼8.12 mg/g, corresponding to specific and residual activity of 537 U/g and 137%, respectively. Fourier transform infrared spectroscopy, thermogravimetric analysis-differential thermogravimetry, field emission scanning electron and atomic force microscopy of RML-CS/CNWs revealed that RML was successfully attached to the surface of crosslinked CS/CNWs. Under an optimized condition, the highest yield of eugenyl benzoate (56.3%) was attained after 5 h using 3 mg/mL of RML-CS/CNWs with molar ratio of eugenol: benzoic acid of 3:1, as compared to only 47.3% for the free RML. Analyses of FTIR and NMR on purified eugenyl benzoate affirmed that the ester was successfully produced in the enzymatic esterification. Therefore, the use of the RML-CS/CNWs biocatalysts appears promising to afford good yields of eugenyl benzoate within a relatively shorter reaction time.
Increasing environmental concerns have led to greater attention to the development of biodegradable materials. The aim of this paper is to investigate the effect of banana leaf fibre (BLF) on the thermal and mechanical properties of thermoplastic cassava starch (TPCS). The biocomposites were prepared by incorporating 10 to 50 wt.% BLF into the TPCS matrix. The samples were characterised for their thermal and mechanical properties. The results showed that there were significant increments in the tensile and flexural properties of the materials, with the highest strength and modulus values obtained at 40 wt.% BLF content. Thermogravimetric analysis showed that the addition of BLF had increased the thermal stability of the material, indicated by higher-onset decomposition temperature and ash content. Morphological studies through scanning electron microscopy (SEM) exhibited a homogenous distribution of fibres and matrix with good adhesion, which is crucial in improving the mechanical properties of biocomposites. This was also attributed to the strong interaction of intermolecular hydrogen bonds between TPCS and fibre, proven by the FT-IR test that observed the presence of O-H bonding in the biocomposite.
The objective of this work was to study the influence of cellulose nanofibrils (CNF) on the physical, mechanical, and thermal properties of Jatropha oil-based waterborne polyurethane (WBPU) nanocomposite films. The polyol to produce polyurethane was synthesized from crude Jatropha oil through epoxidation and ring-opening method. The chain extender, 1,6-hexanediol, was used to improve film elasticity by 0.1, 0.25, and 0.5 wt.% of CNF loading was incorporated to enhance film performance. Mechanical performance was studied using a universal test machine as specified in ASTM D638-03 Type V and was achieved by 0.18 MPa at 0.5 wt.% of CNF. Thermal gravimetric analysis (TGA) was performed to measure the temperature of degradation and the chemical crosslinking and film morphology were studied using Fourier-transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM). The results showed that when the CNF was incorporated, it was found to enhance the nanocomposite film, in particular its mechanical and thermal properties supported by morphology. Nanocomposite film with 0.5 wt.% of CNF showed the highest improvement in terms of tensile strength, Young's modulus, and thermal degradation. Although the contact angle decreases as the CNF content increases, the effect on the water absorption of the film was found to be relatively small (<3.5%). The difference between the neat WPBU and the highest CNF loading film was not more than 1%, even after 5 days of being immersed in water.
Synthesis of nanoparticles by using plant have sparked interest among researchers due to environmentally safe, inexpensive and simple method to compare with chemical method. Use of plant in synthesis zinc oxide nanoparticles (ZnO NPs) that act as reducing and capping agent are more recommended, due to high production of product and rate of synthesis is faster than using microorganism. This study focus on the synthesis of ZnO NPs by using leaf extract of aloe vera (Aloe bardenisis miller) with different concentration (30%, 40% and 50%) and various calcination temperature which are 500 ˚C, 700 ˚C and 900 ˚C for 4 hours. Fourier – transform infrared spectroscopy (FTIR), Thermogravimetric Analysis (TGA), scanning electron microscopy (SEM), X-ray Diffraction (XRD) and Brunauer-Emmet and Teller (BET) were used to characterize the prepared samples. FTIR spectra showed present wavenumber in between 400-500 cm-1 indicated the presence of Zn-O stretch. Powder XRD pattern confirmed the hexagonal wurtzite structure with average particles size from 24.19 nm to 67.69 nm for all concentration and temperature by using Scherer’s equation. For SEM analysis the images show irregular shape for concentrations 30% and 50% with size range from 500 nm to 900 nm while for concentration 40% cubic shape was observe with size range from 140 nm to 900 nm. All characterize show that formation of ZnO NPs depend on the concentration and calcination temperature. Sample 30% and 50% ZnO NPs was applied in lithium battery at voltage from 0.01 to 3. 1.2 mAhg-1 was recorded for sample 30% ZnO NPs while 100 mAhg-1.
Semiconductor oxides such as titanium dioxide (TiO2) and zinc oxide (ZnO) are used as the photocatalyst for removing contaminants. In addition, TiO2 and ZnO nanoparticles in the suspension form makes it difficult to be recovered and recycled. This study was conducted to investigate the efficiency of immobilizing TiO2 and ZnO nanoparticles in epoxy beads. The immobilization process using different ratios of photocatalysts TiO2/ZnO (1:0, 3:1, 1:1, 1:3 and 0:1) fixed on epoxy material. These epoxy beads were used for dye removal in photocatalysis using methylene blue (MB) solution at a concentration of 10mg/L. Besides, epoxy beads also characterized using scanning electron microscope (SEM), attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectroscopy and thermogravimetric analysis (TGA). The results showed that the highly recommended epoxy bead is 3:1 ratio of TiO2/ZnO because it has good performance in dye degradation that proved from reducing concentration of MB to 2.4mg/L (76%). However, TiO2/ZnO characterization of 3:1 by SEM show on the surface the particle are found to be spherical in shape which is relatively high efficiency for the degradation, ATR-FTIR pattern in broad band 4000 cm-1 - 400cm-1 which correspond to hydroxyl stretching to be adsorbed at peak (474.49 cm-1 - 3722.61cm-1) respectively to the optimum for the degradation and TGA rate of change are 5mg to 2.5mg that residue (49.78%) due to decomposition or oxidation from mass loss. These findings are very effective and economical technique to be cost saving and highly efficient photocatalyst.
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.
Lanthanide element in the methanation reaction gives an excellent catalytic performance at low reaction temperature. Praseodymium is one of lanthanide element and was chosen due to its properties which are thermally stable and provide excess of oxygen in the oxide lattice. Therefore, a catalyst of Ru/Mn/Pr (5:30:65)/Al2O3 (RMP, 5:30:65/Al2O3) was prepared via wetness impregnation method and the effect of calcination temperature on the catalyst performance was investigated using FTIR analysis. The RMP/Al2O3 catalyst calcined at 800 o C was chosen as an excel catalyst with CO2 conversion of 96.9% and CH4 formation of 45.1% at 350 o C reaction temperature. From the EDX mapping, it can be observed that the distribution of all element is homogeneous at 800 o C and 900 o C except Ru, O and Al at 1000 o C calcination temperature. The image from FESEM also shows the presence of some crystal shape on the catalyst surface. From the FTIR analysis, the peak stretching and bending mode of O-H bond decreased when the calcination temperature increased.
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.
At present, heavy metal pollution is a major environmental concern and the adsorption technique is a potent method for removal of these heavy metals from wastewater. Activated carbon is one of the best adsorbents for metal ionsremoval but it is sometimes restricted due to high cost and problems with regeneration hamper large scale application. Low cost adsorbent is alternatively being introduced to replace activated carbon since it is available in large quantity, renewable and inexpensive. Hence, Pennisetum purpureum(elephant grass) was investigated for its potential in cadmium ions removal. The adsorbent was characterized by Fourier Transforms Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM), Brunauer–Emmett–Teller (BET) and Barrett–Joyner–Halenda (BJH) analyses.The effects of pH (1 to 5), initial metal ion concentration (5 to 25 mg/L), contact time (10 to 60 minutes) and adsorbent dosage (0.2 to 1.0 g) on cadmium ions removal were conducted by batch adsorption experiments. In this study, the FT-IR results demonstrated that the functional groups for untreated and nitric acid-treated P. purpureum mainly consisted of carbonyl, carboxyl, hydroxyl and amine groups which are able to bind with positively charged cadmium ions. SEM micrographs have proven that nitric acid modification would remove the surface impurities of P. purpureum, which increased the surface roughness, produced deep, open pores and better pore size distribution. From the BET and BJH analyses, the treated P. purpureum was mesoporous, had larger surface area and pore volume compared to untreated P. purpureum. The best pH, adsorbent dosage and contact time were pH 4, 0.6 g and 30 minutes, respectively. The highest removal percentage of cadmium ions for both untreated and treated P. purpureum were 92% and 98% correspondingly. The results shown strengthened the fact that both biosorbents have great potential in cadmium ions removal.
Star-shaped polymers have vast potential in bioapplication due to their architecture. In this study, the suitability of ring opening polymerization (ROP) technique to synthesis star-shaped poly(caprolactone) and the thermal properties of the synthesized star-shaped polymers were demonstrated. The 4 -arm star- shaped of poly(caprolactone) (4s PCL) with -OH terminal and average molecular weight (Mn) of 5000, 10000, and 15000 g/mol were synthesized via ROP of ԑ-caprolactone (ԑ-CL) using a symmetric pentaerythritol (PET) as the core. Different molecular weights were obtained by using different ratios of ԑ-CL and PET in the presence of catalyst, stannous octoate (Sn(Oct)2). The FTIR spectra showed the presence of bands of methylene group of polymer repeating chain which confirm ROP of the ԑ- caprolactone. The average molecular weight (Mn) determined from proton nuclear magnetic resonance (1H NMR) analysis showed that all 4s PCL have approximately the same molecular weight as the theoretical values. All polymers obtained had high yield with >85%. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis showed that there were no significance different in the thermal properties of the synthesized polymers. A single step degradation for all 4s PCL was observed and the crystallization melting point of the polymers was within the range of melting point of PCL.
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.
Introduction: : Ginseng is a type of traditional medicine that has been used for thousand years to treat various dis- eases and has been proven effective in treating cardiovascular diseases. Incorporation of polyaniline (PANI) which is a type of conductive polymer together with ginseng into poly(lactic-co-glycolic acid) (PLGA) microcapsules is neces- sary for the treatment of cardiovascular diseases as the polymer will control drug release and the electroconductivity of PANI is beneficial on myocardium cells. Methods: Therefore, this project involved the encapsulation of ginseng inside PLGA/PANI microcapsules. The encapsulation of ginseng inside the microcapsules was verified through the identification of chemical composition of ginseng, PLGA and PANI using attenuated total reflectance-Fourier trans- form infrared spectroscopy (ATR-FTIR). Results: The results of scanning electron microscope (SEM) showed the formation of microspheres where the microcapsule size was decreased from 3.14±1.87 μm to 1.98±1.30 μm as the concentration of PANI increased. The distribution of microcapsules size was more homogeneous in the high con- centration of PANI as been determined through the histogram analysis. In addition, the fluorescence analysis demon- strated the efficiency of ginseng encapsulation inside PLGA/PANI microcapsules through the appearance of stained ginseng inside the microcapsules. Conclusion: As a conclusion, the ginseng was successfully encapsulated within PLGA/PANI microcapsules that will be beneficial in drug delivery application, specifically in the cardiovascular area.
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.