Nanostructure materials are of interest in last few decades due to their unique size-dependent physio-chemical properties. In this paper, zinc oxide (ZnO) and barium doped ZnO nanodisks (NDs) were synthesized using sonochemical method and characterized by various techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscope (SEM), UV-vis absorption and dielectric measurements. The XRD and FTIR studies confirm the crystalline nature of ZnO NDs, and the average crystallite size was found to be ~25 nm for pure ZnO and ~22 nm for Ba doped ZnO NDs. SEM study confirmed the spherical shaped ZnO NDs with average sizes in the range of 20-30 nm. The maximum absorbance was obtained in the 200-500 nm regions with a prominent peak absorbance were observed by UV-vis spectra. The corresponding band gap for ZnO NDs and Ba doped ZnO NDs were calculated using Tauc's plot and was found to be 3.12 and 3.04, respectively. The conductivity and dielectric measurements as a function of frequency have been studied.
Biosynthesis of nanoparticles has now become a novel trend in addressing some of the environmental issues by adopting eco-friendly approaches in manoeuvring nanoparticles for various applications. Plants and micro-organisms have been the potential sources of the biological mode of synthesizing nanoparticles as part of their bioremediation process. This principle has been harnessed for synthesizing nanoparticles either extra or intracellularly. In this line of phyto-mediated synthesis, eucalyptus buds have been used for synthesizing gold nanoparticles (Au NPs) under optimized laboratory conditions. The UV-visible spectrum of the Au NPs showed typical surface plasmon resonance at 550 nm (λmax) with a crystalline phase measuring <100 nm in size and monodispersed as revealed from XRD, FESEM, and AFM analyses. The biological role of phytochemical concoction in reducing and stabilizing the Au NPs was clearly identified from FT-IR studies. The antimicrobial effect of the Au NPs against clinically important pathogens viz. Staphylococcus sp., Pseudomonas sp., Bacillus sp. and E. coli determined using the disk diffusion method showed no significant antibacterial effect at all concentrations. Cytotoxicity studies were carried using Vero and HEp-2 cell lines and the 50% inhibition concentration (IC50) was determined to be 1.25 mg and 0.625 mg/mL respectively. Au NPs with potential antimicrobial and anti-proliferative effects could found profound implications in the field of nanomedicine once the toxicity in vivo has been investigated.
Ion-imprinting polymers (IIPs) materials draw the great recognition because of the powerful selectivity to the desired metal ions. Therefore, the ion-imprinting polymer (Ce-IIP) was prepared by using cerium metal with amidoxime ligand as the complexing agent, in addition ethylene glycol dimethacrylate (EGDMA) and 2,2-azobisisobutyronitrile (AIBN) are crosslinking agent and free radical initiator, respectively. Aqueous HCl was applied to leach the cerium ions from the imprinted polymer for the creation of cavities of template, which is utilized for further cerium ions adsorption with high selectivity. The Ce-IIP was characterized by using ICP-MS, FE-SEM and also solid state analysis by UV-vis NIR spectroscopy. FT-IR study confirmed the complexation of the Ce-IIP was successful. The optimum pH was found to be 6 and the highest adsorption capacity was estimated about 145 mg g-1. Thus, the prepared Ce-IIP gave very good selectivity to cerium ions in the presence of lanthanide ions and also Ce-IIP can be reused 10 times without a substantial loss in adsorption capacity.
Graphene oxide/Cuprous oxide (GO/Cu₂O) composite is a visible light photocatalyst for the degradation of dyes. A simple and efficient approach for preparing GO/Cu₂O composite adopted in this study involves reducing cuprous oxide precursors in the presence of graphene oxide using an aqueous solution of pulp derived from banana fruit. The GO/Cu₂O composite was characterized by Fourier transform infrared spectroscopy (FT-IR), Diffused reflectance Ultraviolet visible spectroscopy (DRS UV-Vis), Raman spectroscopy and Field Emission Scanning electron microscopy (FE-SEM). Cu₂O particles were distributed randomly on the graphene oxide sheets due to the template effect of GO. The results showed higher photocatalytic activity for the composite (band gap 2.13 eV), for the degradation of the organic dyes (Methylene blue and Rhodamine-B). The enhanced photocatalytic activity is due to effective charge transfer from GO to Cu₂O, and high specific surface area which improves the effective separation of the generated electron-hole pairs. Our present study is inspired by a facile, low cost, green production of (GO/Cu₂O) composite whose photocatalytic activity can be extended to degradation of all other water-born textile dyes.
Au-Ag alloy nanoparticles are physically synthesized using rapid, simple and efficient Q-switched Nd:YAG pulsed laser ablation in liquid technique (PLAL). Au and Ag colloidal solutions are separately prepared by 1064 nm laser ablation of metallic target (gold and silver) which is immersed in deionized water. Au-Ag alloy nanoparticles are prepared by irradiating the mixture of Au and Ag colloidal solutions with 532 nm of second harmonic wavelength of Nd:YAG laser at three different ratio, 3:1, 1:1 and 1:3 within different exposure times. The three of plasmon absorption bands of Au-Ag nanoparticles are shifted linearly to the lower wavelength [499.67 nm (3:1), 481.25 nm (1:1), 467.91 nm (1:3)], as compared to plasmon absorption spectra of pure Au (520 nm) and Ag (400 nm). Moreover, the change in colors are also observed from red (Au) and yellow (Ag) to orange, brown and green color due to the Au-Ag alloy formations, respectively. Transmission electron microscopy shows the Ag shell around the inner core of Au spherical metal with broad size distribution due to the three different volume ratio, respectively (1.7 nm, 0.7 nm, 1.4 nm). Energy-dispersive X-ray spectroscopy analysis confirms the presence of Au and Ag elements in Au-Ag alloy nanoparticles without any contaminations. Attenuated total reflectance fourier transform infrared spectroscopy analysis also confirms the homogenous Au-Ag alloys chemical bonding.
Aluminium substituted cobalt-copper Co1-xCuxFe2-xAlxO₄, (x ═ 0.8) nanoparticles are grown and sintered at different temperature in the range 600 to 900 °C. XRD analysis on nanoparticles prepared at sintered temperatures of 700 °C and 800 °C confirms the spinel structure and presence of hematite phase (alpha ferrite) in them. The dielectric behaviour of the prepared nano-particles is investigated. Although crystallinity improved with increase in sintering temperature and there was a dielectric loss at higher probe analyser frequency. The synthesized nanoparticles an average particle size of 20-24 nm while the FTIR absorption in regions of 586-595 cm-1 and 450-460 cm-1 indicated the presence of intrinsic vibrations of the tetrahedral and octahedral complexes respectively. Electrical resistivity as a function of temperature confirms the semiconducting nature of the Cu-Al substituted cobalt ferrite, and is attributed to the hopping mechanism between Fe2+ Fe3+ ions and Co2+ Cu2+, Co2+ Al3+. The lower values of dielectric constants and dielectric losses make Al-Cu doped cobalt ferrite, a potential material for microwave and radio wave absorber applications.
Recently, the graphite based materials have gained interest as excellent platforms to remove aqueous pollutants via adsorption routes. This is given that such materials possess large specific surface area and low density. In the present work, a comparative study of two facile and effective approaches is conventional thermal heating and microwave irradiation methods to fabricate expanded graphite from available flake graphite sources of Vietnam for oil-contaminated water purification. The as-prepared expanded graphite was characterized by using FT-IR, SEM, XRD and BET analysis. The results exhibited that expanded graphite has multilevel pore structures and the surface area of expanded graphite obtained from microwave irradiation and conventional heating was 147.5 (m²/g) and 100.97 (m²/g) under optimal processing conditions. The as-synthesized expanded graphite from the microwave irradiation method was found to have higher adsorption capacities for diesel oil, crude oil, and fuel oil compared to conventional heating method.
This work is aimed to develop a biocompatible, bactericidal and mechanically stable biomaterial to overcome the challenges associated with calcium phosphate bioceramics. The influence of chemical composition on synthesis temperature, bioactivity, antibacterial activity and mechanical stability of least explored calcium silicate bioceramics was studied. The current study also investigates the biomedical applications of rankinite (Ca3Si2O7) for the first time. Sol-gel combustion method was employed for their preparation using citric acid as a fuel. Differential thermal analysis indicated that the crystallization of larnite and rankinite occurred at 795 °C and 1000 °C respectively. The transformation of secondary phases into the desired product was confirmed by XRD and FT-IR. TEM micrographs showed the particle size of larnite in the range of 100-200 nm. The surface of the samples was entirely covered by the dominant apatite phase within one week of immersion. Moreover, the compressive strength of larnite and rankinite was found to be 143 MPa and 233 MPa even after 28 days of soaking in SBF. Both samples prevented the growth of clinical pathogens at a concentration of 2 mg/mL. Larnite and rankinite supported the adhesion, proliferation and osteogenic differentiation of hBMSCs. The variation in chemical composition was found to influence the properties of larnite and rankinite. The results observed in this work signify that these materials not only exhibit faster biomineralization ability, excellent cytocompatibility but also enhanced mechanical stability and antibacterial properties.
Crystallinity plays a vital role in the pharmaceutical industry. It affects drug manufacturing, development processes, and the stability of pharmaceutical dosage forms. An objective of this study was to measure and analyze the carbamazepine (CBZ) crystallinity before and after formulation. Moreover, it intended to determine the extent to which the crystallinity of CBZ would affect the drug loading, the particle size, and the release of CBZ from the microparticles. The CBZ microparticles were prepared by encapsulating CBZ in ethyl cellulose (EC) polymer using a solvent evaporation method. EC was used here as a release modifier polymer and polyvinyl alcohol (PVA) as an aqueous phase stabilizer. Factorial design was used to prepare the CBZ microparticle formulations, including polymer concentration, solvent (dichloromethane, ethyl acetate), PVA concentrations factor, the homogenization time, and homogenization speed. The crystallinity of CBZ was calculated utilizing differential scanning calorimetry (DSC) thermal analysis. The crystallinity was calculated from the enthalpy of CBZ. Enthalpy was analyzed from the area under the curve peak of CBZ standard and CBZ-loaded microparticles. DSC and ATR-FTIR assessed the possible interaction between CBZ and excipients in the microparticle. The prepared CBZ microparticles showed various changes in the crystallinity rate of CBZ. The changes in the rate of CBZ crystallinity had different effects on the particle size, the drug loading, and the release of CBZ from the polymer. Statistically, all studied factors significantly affected the crystallinity of CBZ after formulation to microparticles.
Ceramic materials play key role in several biomedical applications. One of them is bone graft which is use in treating bone defect which caused by injury or osteoporosis. Calcium phosphates based ceramic are preferred as bone grafts in hard tissue engineering because of their chemical compositions are similar to the composition of human bone, superior bioresorbable and bioactivity. In this study, β-tricalcium phosphate (β-TCP) ceramic was synthesized by using sol-gel method. Phosphorous pentoxide (P2O5) and calcium nitrate tetrahydrate (Ca(NO3)2.4H2O) were used as calcium and phosphate precursors. The effects of calcination temperature on the synthesis powder were studied using the XRD, SEM-EDS and FTIR techniques. It was found that calcination temperature greatly influence the purity of the synthesized powders. The β-TCP was the dominant phase with the formation of α-TCP at calcination temperature from 600 to 800°C. Pure β-TCP was obtained at calcination of 900°C. As the temperature increased to 1000°C, the β-TCP was decomposed to for calcium phosphate oxide (CPO). The sol-gel method has some advantages over other methods, mainly its simplicity and ability to produce pure β-TCP at lower calcination temperature.
In this study, we evaluated and characterized microbial cellulose produced from Kombucha after eighth day of fermentation by employing SEM, FTIR, X-ray diffractometry, adsorption isotherm, and by measuring the swelling properties. Results on SEM revealed microbial cellulose layer to be composed of a compact cellulose ultrafine network like structure. FTIR spectra showed the presence of a characteristic region of anomeric carbons (960 – 730 cm-1), wherein a band at 891.59 cm-1 confirmed the presence of β, 1-4 linkages. Results of FTIR spectra also showed microbial cellulose to be free from contaminants such as lignin or hemicellulose, which are often present in plant cellulose. X-ray diffraction studies exhibited the overall degree of crystallinity index for MCC to be slightly lower than that of microbial cellulose. Results on swelling properties indicated microbial cellulose to possess higher fiber liquid retention values (10-160%) compared to commercial MCC (5-70%). The adsorption isotherm curves showed similarities between microbial cellulose with that of pure crystalline substance. Overall, results obtained in this study were comparable with the commercial microcrystalline cellulose, indicating that the process developed by us can be explored industrially on a pilot scale.
The aim of this work is to study the effect of hydrocolloids; guar gum (GG), xanthan gum (XG) and carboxymethyl cellulose (CMC) on the physicochemical properties, microbiological quality and sensory properties in order to investigate the potential of applying fermented cassava (tapai ubi) in ice cream. Fermented cassava ice cream (FCI) incorporated with the three types of hydrocolloid was prepared and the protein content, pH value, overrun, colour, hardness, microstructure, FTIR spectrum and sensory acceptance of all samples were determined. Fermented cassava ice cream incorporated with XG showed the highest protein content (14.88%), pH value (pH 6.07), and overrun value (4.27%) as compared to the fermented cassava ice cream incorporated with GG and CMC. Meanwhile, ice cream incorporated with GG possessed the highest L* (94.43) and hardness (3693.15 g) value as compared to XG and CMC. The microstructure study showed that the difference in uniformity at the interface obtained with different types of the hydrocolloids added demonstrated the effect of fat absorption at the air interfaces. The FTIR spectrum investigated indicated that the addition of the fermented cassava to FCI had increased the OH group in the ice cream as compared to the control. All samples were microbial safe as the total plate counts in all samples were below the standard as prescribed in Food Act 1983 with no presence of E. coli . In conclusion, fermented cassava ice cream with XG showed the good quality in terms of its pH value, overrun, total plate count and overall acceptability.
Pepsin-solubilized collagen (PSC) was extracted from the body wall of crown-of-thorns starfish (COTS) (Acanthaster planci) using pepsin digestion in 0.5 M acetic acid. The electrophoretic pattern of PSC showed that it consisted of two α chains (α1 and α2 chains). In addition, the peptide mapping showed that there were some differences in peptide patterns among PSC, calf skin collagen and salmon skin collagen. This suggested that the primary structure of the PSC was different from calf skin collagen and salmon skin collagen. Furthermore, Fourier transform infrared spectroscopy (FTIR) investigation showed the existence of triple helical structure in PSC, suggesting that the triple helical structure was well preserved during the extraction of collagen from COTS. The denaturation temperature of PSC was 33.0°C, which was comparable with mammalian collagen. In addition, the amino acid composition analysis showed that the imino acid content of PSC was similar to mammalian collagen but it was higher than other marine collagen. This suggested that the imino acid content might contributed the denaturation temperature of collagen. The results in this study suggest that PSC from the underutilized COTS has potential to be exploited in various commercial applications.
In this study, chitosan/polyvinyl alcohol (PVA)/zeolite nanofibrous composite membrane was fabricated via electrospinning. First, crude chitosan was hydrolyzed with NaOH for 24h. Afterward, hydrolyzed chitosan solution was blended with aqueous PVA solution in different weight ratios. Morphological analysis of chitosan/PVA electrospun nanofiber showed a defect-free nanofiber material with 50:50 weight ratio of chitosan/PVA. Subsequently, 1wt.% of zeolite was added to this blended solution of 50:50 chitosan/PVA. The resulting nanofiber was characterized with field emission scanning electron microscopy, X-Ray diffraction, Fourier transform infrared spectroscopy, swelling test, and adsorption test. Fine, bead-free nanofiber with homogeneous nanofiber was electrospun. The resulting membrane was stable in distilled water, acidic, and basic media in 20 days. Moreover, the adsorption ability of nanofibrous membrane was studied over Cr (VI), Fe (III), and Ni (II) ions using Langmuir isotherm. Kinetic parameters were estimated using the Lagergren first-order, pseudo-second-order, and intraparticle diffusion kinetic models. Kinetic study showed that adsorption rate was high. However, the resulting nanofiber membrane showed less adsorption capacity at high concentration. The adsorption capacity of nanofiber was unaltered after five recycling runs, which indicated the reusability of chitosan/PVA/zeolite nanofibrous membrane. Therefore, chitosan/PVA/zeolite nanofiber can be a useful material for water treatment at moderate concentration of heavy metals.
Many attempts have been focused in the past on preparing of synthetic E-tricalcium (E-TCP), which being employed as bone substitute due to its biocompatibility and resorbability. Low temperature synthesize such as sol-gel method become popular due to the high product purity and homogenous composition. Sol-gel method is less economical towards commercialization because the cost of raw materials and the yield of the product that can be achieved. This paper describes the synthesis of ETCP via mixing of CaCO3 and H3PO4 followed by calcinations process at 750qC – 1050qC. X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimeter (DSC), fourier transformation infra-red (FTIR) were used for characterization and evaluation of the phase composition, morphology, particle size and thermal behavior of the product. E-TCP phase start to occur after calcinations at 750qC.
The present study was carried out to characterize red fruit (Pandanus conoideus Lam) oil (RFO) in term of FTIR spectra, fatty acid composition, and volatile compounds. FTIR spectrum of RFO was slightly
different from other common vegetable oils and animal fats, in which in the frequency range of 1750 – 1700 cm-1, RFO appear two bands. The main fatty acid composition of RFO is oleic acid accounting for 68.80% followed by linoleic acid with the concentration of 8.49%. The main volatile compounds of RFO as determined using gas chromatography coupled with mass spectrometry (GC-MS) and headspace analyser are 1,3-dimethylbenzene (27.46%), N-glycyl- L-alanine (17.36%), trichloromethane (15.22%), and ethane (11.43%).
Multiwall carbon nanotubes (MWCNTs) were synthesized using a tubular microwave chemical vapor deposition technique, using acetylene and hydrogen as the precursor gases and ferrocene as catalyst. The novel MWCNT samples were tested for their performance in terms of Pb(II) binding. The synthesized MWCNT samples were characterized using Fourier Transform Infrared (FT-IR), Brunauer, Emmett and Teller (BET), Field Emission Scanning Electron Microscopy (FESEM) analysis, and the adsorption of Pb(II) was studied as a function of pH, initial Pb(II) concentration, MWCNT dosage, agitation speed, and adsorption time, and process parameters were optimized. The adsorption data followed both Freundlich and Langmuir isotherms. On the basis of the Langmuir model, Qmax was calculated to be 104.2mg/g for the microwave-synthesized MWCNTs. In order to investigate the dynamic behavior of MWCNTs as an adsorbent, the kinetic data were modeled using pseudo first-order and pseudo second-order equations. Different thermodynamic parameters, viz., ∆H(0), ∆S(0) and ∆G(0) were evaluated and it was found that the adsorption was feasible, spontaneous and endothermic in nature. The statistical analysis revealed that the optimum conditions for the highest removal (99.9%) of Pb(II) are at pH5, MWCNT dosage 0.1g, agitation speed 160r/min and time of 22.5min with the initial concentration of 10mg/L. Our results proved that microwave-synthesized MWCNTs can be used as an effective Pb(II) adsorbent due to their high adsorption capacity as well as the short adsorption time needed to achieve equilibrium.
UV-curable hyperbranched urethane acrylate (HBPUA) from oleic acid of palm oil has been synthesized through a medium aided by p-toluene sulfonic acid as a catalyst. This mixture was then used as the core (HBP) and reacted with palm oil oleic acid to form the hyperbranched polyol (HBP-1). HBPUA was prepared by reacting HBP-1 resin with diisocyanate and hydroxyl-containing acrylate monomer with the presence of 0.1-2 wt% dibutyltin dilaurate as a catalyst. The reaction was confirmed by several analytical data i.e. hydroxyl value (OHV), Fourier Transform infrared (FTIR) spectroscopy, gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) spectroscopy analyses. The HBPUA was easily curable when subjected to ultraviolet (UV) radiation.
Six new Pd(II) and Ni(II) metal complexes of N, O-bidentate (L1, L2) and ONNO-tetradentate (L3) Schiff base ligands have been synthesized. The compounds were characterized via various physicochemical and spectroscopic techniques namely elemental analysis (CHN), FT-IR, 1H and 13C NMR as well as magnetic susceptibility measurement. All complexes showed diamagnetism indicating that they are square planar complexes. Catalytic performance of Pd(L1)2 and Pd(L2)2 were investigated for Heck cross-coupling reaction under optimum operating parameters, monitored using GC-FID for 6 h of reaction time in inert conditions. High catalytic activities of up to 90% were observed in the presence of triethylamine as base and DMA as solvent at 100oC with 1 mmol% catalyst loading. The mechanism of catalyzed Heck reaction is proposed to go through a series of conversion of Pd(0)/Pd(II).
The aims of this study are to report on the extraction and characterization of Asian swamp eel (Monopterus albus) skin gelatin. The characterization conducted were includes chemical composition, pH, gel strength, viscosity, thermal property, color and structure determination of extracted eel skin gelatin. Eel skin contains 70.28% moisture, 11.07% protein, 4.21% fat, and 5.01% ash. The chemical composition of eel skin gelatin (yield of 12.75%) was 18.8% moisture, 67.64% protein, 0.34% fat and 1.08% ash, with a pH of 4.62 and gel strength of 215.96 g (± 9.62 g). Although viscosity (2.8 cPa/min) profile of eel skin gelatin showed lower than that of bovine gelatin, the higher melting temperature (35 °C) of eel skin gelatin indicating its higher stability than bovine gelatin with FTIR spectrum similar to that of typical bovine gelatin. Eel skin gelatin has a 71.4 (± 1.14), a +3.2 (± 0.29), and a +7.52 (± 0.29) for L*, a* and b* value respectively, indicate a darker and less yellow colour. These findings show promising potential for the application of eel skin gelatin as an alternative to commercial gelatin.