In this work, sensitive detection of dengue virus type 2 E-proteins (DENV-2 E-proteins) was performed in the range of 0.08 pM to 0.5 pM. The successful DENV detection at very low concentration is a matter of concern for targeting the early detection after the onset of dengue symptoms. Here, we developed a SPR sensor based on self-assembled monolayer/reduced graphene oxide-polyamidoamine dendrimer (SAM/NH2rGO/PAMAM) thin film to detect DENV-2 E-proteins. Surface characterizations involving X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) confirms the incorporation of NH2rGO-PAMAM nanoparticles in the prepared sensor films. The specificity, sensitivity, binding affinity, and selectivity of the SPR sensor were then evaluated. Results indicated that the variation of the sensing layer due to different spin speed, time incubation, and concentration provided a better interaction between the analyte and sensing layer. The linear dependence of the SPR sensor showed good linearity (R2 = 0.92) with the lowest detection of 0.08 pM DENV-2 E-proteins. By using the Langmuir model, the equilibrium association constant was obtained at very high value of 6.6844 TM-1 (R2 = 0.99). High selectivity of the SPR sensor towards DENV-2 E-proteins was achieved in the presence of other competitors.
This study investigates the preliminary efficacy of drug encapsulation in chitosan hydrogels by cathodic electrodeposition for the encapsulation of the aromatic dye methyl orange to enhance drug delivery in biological systems. Chitosan, a biocompatible and transparent polymer, is known for its ability to effectively encapsulate and transport therapeutic agents, which is critical for sustained and targeted drug release. Methyl orange was selected as a model drug to study the effects of deposition and immersion times on encapsulation efficiency. The effects of deposition and immersion times on encapsulation efficiency were analyzed by synthesizing multilayer hydrogels via electrochemical oxidation. Characterization techniques, including UV-visible spectroscopy, FTIR, and NMR, were employed; FTIR indicated an effective absorption of 4.34 % for Td50Ti60, while UV-Vis showed 46.41 % at Td60Ti50. NMR analysis revealed effective concentrations of 0.47 mM for Td70Ti60 and 0.38 mM for Td60Ti50, indicating that longer immersion times enhance absorption. These findings provide a foundation for further studies aimed at optimizing drug delivery strategies and improving the therapeutic efficacy of encapsulated agents in biological applications.
This study describes the synthesis, characterization and application of a new chrysin-based silica core-shell magnetic nanoparticles (Fe3O4@SiO2-N-chrysin) as an adsorbent for the preconcentration of Cu(II) from aqueous environment. The morphology, thermal stability and magnetic property of Fe3O4@SiO2-N-chrysin were analyzed using FTIR, FESEM, TEM, XRD, thermal analysis and VSM. The extraction efficiency of Fe3O4@SiO2-N-chrysin was analyzed using the batch wise method with flame atomic absorption spectrometry. Parameters such as the pH, the sample volume, the adsorption-desorption time, the concentration of the desorption solvent, the desorption volume, the interference effects and the regeneration of the adsorbent were optimized. It was determined that Cu(II) adsorption is highly pH-dependent, and a high recovery (98%) was achieved at a pH 6. The limit of detection (S/N=3), the limit of quantification (S/N=10), the preconcentration factor and the relative standard deviation for Cu(II) extraction were 0.3 ng mL(-1), 1 ng mL(-1), 100 and 1.9% (concentration=30 ng mL(-1), n=7), respectively. Excellent relative recoveries of 97-104% (%RSD<3.12) were achieved from samples from a spiked river, a lake and tap water. The MSPE method was also validated using certified reference materials SLRS-5 with good recovery (92.53%).
Partially phosphorylated polyvinyl alcohol (PPVA) with aluminum phosphate (ALPO4) composites was synthesized by solution casting technique to produce (PPVA)(100-y) - (ALPO4)(y) (y = 0, 1, and 2). The surface structure and thermal properties of the films were characterized using Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). The results showed that the films have higher thermal stability with strong bonding between PPVA and ALPO4.
The [Co(naphophen)(PPh3)(OH2)]ClO4 and [Co(naphophen)(PBu3)(OH2)]BF4 (where naphophen=bis(naphthaldehyde)1,2-phenylenediimine) complexes were synthesized and chracterized by FT-IR, UV-Vis, (1)H NMR, (13)C NMR spectroscopy and elemental analysis techniques. The coordination geometry of the synthesized complexes were determined by X-ray crystallography. Cobalt (III) complexes have six-coordinated pseudo-octahedral geometry in which the O(1), O(2), N(1) and N(2) atoms of the Schiff base forms the equatorial plane. These complexes showed a dimeric structure via hydrogen bonding between the phenolate oxygen and the hydrogens of the coordinated H2O molecule. The theoretical calculations were also performed to optimize the structure of the complexes in the gas phase to confirm the structures proposed by X-ray crystallography. In addition, UV-Visible and IR spectra of complexes were calculated and compared with the corresponding experimental spectra to complete the experimental structural identification. The synthesized complexes were incorporated onto the Montmorillonite-K10 nanoclay via simple ion-exchange reaction. The structure and morphology of the obtained nanohybrids were identified by FT-IR, XRD, TGA/DTA, SEM and TEM techniques. Based on the XRD results of the new nanohybrid materials, the Schiff base complexes were intercalated in the interlayer spaces of clay. SEM and TEM micrographs of the clay/complex shows that the resulting hybrid nanomaterials has layer structures.
Developing novel fish gelatin films with better mechanical properties than mammalian gelatin is a challenging but promising endeavor. Studies were undertaken to produce fish gelatin films by combining treatments with different sugars (ribose and lactose) followed 'by' 'and' ultraviolet (UV) radiation, as possible cross-linking agents. Increase in tensile strength and percent elongation at break was recorded, which was more significant in films without sugars that were exposed to UV radiation. Films with added ribose showed decreased solubility after UV treatment and exhibited higher swelling percentage than films with added lactose, which readily dissolved in water. FTIR spectra of all the films showed identical patterns, which indicated no major changes to have occurred in the functional groups as a result of interaction between gelatin, sugars and UV irradiation. The results of this study could be explored for commercial use, depending on industrial needs for either production of edible films or for food packaging purposes.
Anode biofilm is a crucial component in microbial fuel cells (MFCs) for electrogenesis. Better knowledge about the biofilm development process on electrode surface is believed to improve MFC performance. In this study, double-chamber microbial fuel cell was operated with diluted POME (initial COD = 1,000 mg L(-1)) and polyacrylonitrile carbon felt was used as electrode. The maximum power density, COD removal efficiency and Coulombic efficiency were found as 22 mW m(-2), 70 and 24 %, respectively. FTIR and TGA analysis confirmed the formation of biofilm on the electrode surface during MFC operation. The impact of anode biofilm on anodic polarization resistance was investigated using electrochemical impedance spectroscopy (EIS) and microbial community changes during MFC operation using denaturing gradient gel electrophoresis (DGGE). The EIS-simulated results showed the reduction of charge transfer resistance (R ct) by 16.9 % after 14 days of operation of the cell, which confirms that the development of the microbial biofilm on the anode decreases the R ct and therefore improves power generation. DGGE analysis showed the variation in the biofilm composition during the biofilm growth until it forms an initial stable microbial community, thereafter the change in the diversity would be less. The power density showed was directly dependent on the biofilm development and increased significantly during the initial biofilm development period. Furthermore, DGGE patterns obtained from 7th and 14th day suggest the presence of less diversity and probable functional redundancy within the anodic communities possibly responsible for the stable MFC performance in changing environmental conditions.
Biochar has received great attention recently due to its potential to improve soil fertility and immobilize contaminants as well as serving as a way of carbon sequestration and therefore a possible carbon sink. In this work, a series of biochars were produced from empty fruit bunch (EFB) and rice husk (RH) by slow pyrolysis at different temperatures (350, 500, and 650°C) and their physicochemical properties were analysed. The results indicate that porosity, ash content, electrical conductivity (EC), and pH value of both EFB and RH biochars were increased with temperature; however, yield, cation exchange capacity (CEC), and H, C, and N content were decreased with increasing pyrolysis temperature. The Fourier transform IR spectra were similar for both RH and EFB biochars but the functional groups were more distinct in the EFB biochar spectra. There were reductions in the amount of functional groups as pyrolysis temperature increased especially for the EFB biochar. However, total acidity of the functional groups increased with pyrolysis temperature for both biochars.
Carbon nanotubes-mesostructured silica nanoparticles (CNT-MSN) composites were prepared by a simple one step method with various loading of CNT. Their surface properties were characterized by XRD, N2 physisorption, TEM and FTIR, while the adsorption performance of the CNT-MSN composites were evaluated on the adsorption of methylene blue (MB) while varying the pH, adsorbent dosage, initial MB concentration, and temperature. The CNTs were found to improve the physicochemical properties of the MSN and led to an enhanced adsorptivity for MB. N2 physisorption measurements revealed the development of a bimodal pore structure that increased the pore size, pore volume and surface area. Accordingly, 0.05 g L(-1) CNT-MSN was able to adsorb 524 mg g(-1) (qm) of 60 mg L(-1) MB at pH 8 and 303 K. The equilibrium data were evaluated using the Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich isotherm models, with the Langmuir model affording the best fit to the adsorption data. The adsorption kinetics were best described by the pseudo-first order model. These results indicate the potential of CNT-MSN composites as effective new adsorbents for dye adsorption.
2-(4-Chlorophenyl)-2-oxoethyl 3-methylbenzoate is synthesized by reacting 4-chlorophenacyl bromide with 2-methylbenzoic acid using a slight excess of potassium or sodium carbonate in DMF medium at room temperature. The structure of the compound was confirmed by IR and single-crystal X-ray diffraction studies. FT-IR spectrum of 2-(4-chlorophenyl)-2-oxoethyl-3-nitrobenzoate was recorded and analyzed. The crystal structure is also described. The vibrational wavenumbers were computed using HF and DFT methods and are assigned with the help of potential energy distribution method. The first hyperpolarizability and infrared intensities are also reported. The geometrical parameters of the title compound obtained from XRD studies are in agreement with the calculated (DFT) values. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. The HOMO and LUMO analysis are used to determine the charge transfer within the molecule. MEP was performed by the DFT method.
Ag/PMMA nanocomposites were successfully synthesized by in-situ technique. Transmission electron microscopy (TEM) images show that the particles are spherical in shape and their sizes are dependent on temperature. The smallest particle achieved high stability as indicated from Zeta sizer analysis. The red shift of surface plasmon resonance (SPR) indicated the increases of particle sizes. X-ray diffraction (XRD) patterns exhibit a two-phase (crystalline and amorphous) structure of Ag/PMMA nanocomposites. The complexation of Ag/PMMA nanocomposites was confirmed using Raman spectroscopy. Fourier transform infrared spectroscopy spectra confirmed that the bonding was dominantly influenced by the PMMA and DMF solution. Finally, thermogravimetric analysis (TGA) results indicate that the total weight loss increases as the temperature increases.
As Malaysia is one of the world's largest producer of palm oil, large amounts of palm oil mill effluent (POME) is generated. It was found that negatively charged components are accountable for POME color. An attempt was made to remove residual contaminants after conventional treatment using anion base resin. Adsorption experiments were carried out in fixed bed column. Various models such as the Thomas, the Yoon-Nelson, the Wolborska and BDST model were used to fit the experimental data. It was found that only the BDST model was fitted well at the initial breakthrough time. A wavelet neural network model (WNN) was developed to model the breakthrough curves in fixed bed column for multicomponent system. The results showed that the WNN model described breakthrough curves better than the commonly used models. The effects of pH, flow rate and bed depth on column performance were investigated. It was found that the highest uptake capacity was obtained at pH 3. The exhaustion time appeared to increase with increase in bed length and decrease in flow rate.
Perovskite-structured lead titanate thin films have been grown on FTO-coated glass substrates from a single-source heterometallic molecular complex, [PbTi(μ2-O2CCF3)4(THF)3(μ3-O)]2 (1), which was isolated in quantitative yield from the reaction of tetraacetatolead(IV), tetrabutoxytitanium(IV), and trifluoroacetic acid from a tetrahydrofuran solution. Complex 1 has been characterized by physicochemical methods such as melting point, microanalysis, FTIR, (1)H and (19)F NMR, thermal analysis, and single-crystal X-ray diffraction (XRD) analysis. Thin films of lead titanate having spherical particles of various sizes have been grown from 1 by aerosol-assisted chemical vapor deposition at 550 °C. The thin films have been characterized by powder XRD, scanning electron microscopy, and energy-dispersive X-ray analysis. An optical band gap of 3.69 eV has been estimated by UV-visible spectrophotometry.
Novel ionophores comprising various hydroxide and amine structures were immobilized onto poly(vinyl chloride) (PVC) matrices, and these were examined to determine Ti(III) selectivity. To predict the selectivity of Ti(III), a PVC membrane was used to investigate the binding of Ti(III) to c-methylcalix[4]resorcinarene (CMCR). The study showed that the chelating ligand, CMCR, was coordinated selectively to Ti(III) at eight coordination sites involving the oxygen atoms at the interface of the membrane/solution. The membrane was prepared, based on CMCR as an ionophore, sodium tetrakis(4-fluorophenyl) borate (NaTFPB) as a lipophilic ionic additive, and dioctylphthalate (DOP) as a plasticizer. The immobilization of the ionophore and surface characterization studies revealed that the performance of CMCR-immobilized PVC was equivalent to that of mobile ionophores in supported liquid membranes (SLMs). The strengths of the ion-ionophore (CMCR-Ti(OH)(OH(2))(5) (2+)) interactions and the role of ionophores on membranes were studied via UV-Vis, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and and X-ray diffraction (XRD).
Heavy metal oxide glasses, containing bismuth and/or lead in their glass structure are new alternatives for rare eart (RE) doped hosts. Hence, the study of the structure of these vitreous systems is of great interest for science and technology. In this research work, GeO(2)-PbO-Bi(2)O(3) glass host doped with Er(3+)/Yb(3+) ions was synthesized by a conventional melt quenching method. The Fourier transform infrared (FTIR) results showed that PbO and Bi(2)O(3) participate with PbO(4) tetragonal pyramids and strongly distort BiO(6) octahedral units in the glass network, which subsequently act as modifiers in glass structure. These results also confirmed the existence of both four and six coordination of germanium oxide in glass matrix.
The Cr(III) sorption experiments onto Kappaphycus alvarezii waste biomass were conducted at different pH values (2-6) under the conditions of initial metal concentration of 10-50 mg/L and the chemical compositions of Cr-Cu and Cr-Cd. The Cr(III) sorption capacities were slightly dependent on pH, and the maximum sorption capacity was 0.86 mg/g at pH 3. The sorption capacities increased with increase in the initial metal concentration, whereas it was suppressed by the presence of Cu(II) and Cd(III) in the solution. The Cr(III) sorption equilibrium was evaluated using Langmuir, Freundlich and BET isotherms. The sorption mechanisms were characterised using scanning electron microscopy and Fourier transform infrared spectroscopy. The main mechanisms were ion exchange coupled with a complexation mechanism. Kappaphycus alvarezii waste biomass represents a potential for Cr(III) ion removal from aqueous solution.
Sunflower seed oil residue, a by-product of sunflower seed oil refining, was utilized as a feedstock for preparation of activated carbon (SSHAC) via microwave induced K(2)CO(3) chemical activation. SSHAC was characterized by Fourier transform infrared spectroscopy, nitrogen adsorption-desorption and elemental analysis. Surface acidity/basicity was examined with acid-base titration, while the adsorptive properties of SSHAC were quantified using methylene blue (MB) and acid blue 15 (AB). The monolayer adsorption capacities of MB and AB were 473.44 and 430.37 mg/g, while the Brunauer-Emmett-Teller surface area, Langmuir surface area and total pore volume were 1411.55 m(2)/g, 2137.72 m(2)/g and 0.836 cm(3)/g, respectively. The findings revealed the potential to prepare high surface area activated carbon from sunflower seed oil residue by microwave irradiation.
Silver nanoparticles were fabricated by ablation of a pure silver plate immersed in castor oil. A Nd:YAG-pulsed Q-switch laser with 1064-nm wavelength and 10-Hz frequency was used to ablate the plate for 10 minutes. The sample was characterized by ultraviolet-visible, atomic absorption, Fourier transform-infrared spectroscopies, and transmission electron microscopy. The results of the fabricated sample showed that the nanoparticles in castor oil were about 5-nm in diameter, well dispersed, and showed stability for a long period of time.
The aim of this study was to explore the utilization of polymeric membrane for bio-sensing application in most efficient and rapid way. Customization of membrane formulation via phase separation study to modify its morphologies and properties enable the detection of different pathogens in a specific manner. Experimental findings (FESEM, through-pore distribution, porosity, capillary flow test and protein binding test) verified the predictions of faster capillary flow time and higher membrane's protein binding by the addition of cellulose acetate and nitrocellulose to the membrane casting dope, respectively. Throughout the phase separation study, the potential phase behavior was investigated, which was correlating various membrane structures to its performances for potential pathogens detection in water.
A series of 5-substituted-4-amino-1,2,4-triazole-3-thioesters was synthesized by converting variously substituted organic acids successively into the corresponding esters, hydrazides, 5-substituted-1,3,4-oxadiazole-2-thiols, 5-substituted-1,2,4-triazole-2-thiols and 5-substituted-1,3,4-oxadiazole-2-thioesters. Finally the target compounds were obtained by refluxing 5-substituted-1,3,4-oxadiazole-2-thioesters in the presence of hydrazine hydrate and absolute alcohol. The structures of the synthesized compounds were established by physicochemical and spectroscopic methods. The synthesized compounds were evaluated for their in vitro antifungal activity. Some of the evaluated compounds possessed significant antifungal activity as compared to a terbinafine standard.