β-tricalcium phosphate (β-TCP) powders were synthesized by using various particles sizes (40 nm – 780 μm) calcium carbonate (CaCO3) and phosphoric acid (H3PO4) at room temperature (25 ˚C). The synthesized powders were characterized by using X-Ray Diffraction (XRD) method. The purity of β-TCP powders were determined from XRD pattern while the crystallite size of β-TCP powders were calculated by using Scherrer equation. Results shows that the purity of β-TCP powders were ranged from 20.33 % to 81.94 % while the crystallite size of β- TCP powders were ranged from 0.04391 μm to 0.06751 μm. From this work, particle size of CaCO3 will influenced the purity but not the mean crystallite size of synthesized β-TCP.
Indialite or α-cordierite was synthesized by glass crystallization method using mainly talc and kaolin and with small amount of MgO, Al2O3, SiO2 to compensate the chemical formulation of non-stoihiometric compositions of cordierite. (3MgO.1.5Al2O3.5SiO2). B2O3, P2O5 and CaO was also added to decrease the melting and sintering temperature of cordierite. The glasses were pelletized and sintered from 850 o C up to 1050 o C. Phase compositions of both heat treated glass was quantified by X-ray powder diffraction data by the Rietveld method using TOPAS Ver 3 software. Result shows that about 60wt% of α cordierite has successfully crystallized at 850 o C. Beside secondary phases (forsterite) which come from initial raw materials, phases from grinding media were also presents in the sample. The contamination was considered high since it has reacted with existence phases to form a new phase at higher temperature. Without any contamination from grinding it was expected to obtain more than 90wt% α cordierite using the same composition.
Hydroxyapatite (HA) has been earmarked as suitable for implantation within the human of its chemical makeup to human bone. In this paper, HA powders were synthesized via the precipitation method where phosphoric acid (H3PO4) was titrated into calcium hydroxide solution [Ca(OH)2]. Two parameters such as temperature and stirring rate were identified as factors that influenced the amount and purity of HA powder. Phase identification of the synthesized powder was done using X-Ray Diffraction (XRD). The results show that HA phase can be synthesized from this titration process of Ca(OH)2 and H3PO4 with yield amount of HA powder around 45 - 61 grams but with less than hundred percent purity. In order to study the effect of heat treatment to HA crystals structure, HA powder was calcined at 850 degrees C for 2 hours. It's found that the degree of crystallinity increases after calcination because of lattice expansion when the materials were heated at higher temperature
We report on a recycling project in which α-Al(2)O(3) was produced from aluminum cans because no such work has been reported in literature. Heated aluminum cans were mixed with 8.0 M of H(2)SO(4) solution to form an Al(2)(SO(4))(3) solution. The Al(2)(SO(4))(3) salt was contained in a white semi-liquid solution with excess H(2)SO(4); some unreacted aluminum pieces were also present. The solution was filtered and mixed with ethanol in a ratio of 2:3, to form a white solid of Al(2)(SO(4))(3)·18H(2)O. The Al(2)(SO(4))(3)·18H(2)O was calcined in an electrical furnace for 3 h at temperatures of 400-1400 °C. The heating and cooling rates were 10 °C /min. XRD was used to investigate the phase changes at different temperatures and XRF was used to determine the elemental composition in the alumina produced. A series of different alumina compositions, made by repeated dehydration and desulfonation of the Al(2)(SO(4))(3)·18H(2)O, is reported. All transitional alumina phases produced at low temperatures were converted to α-Al(2)O(3) at high temperatures. The X-ray diffraction results indicated that the α-Al(2)O(3) phase was realized when the calcination temperature was at 1200 °C or higher.
A systematic set of borotellurite glasses doped with manganese (1-x) [(B(2)O(3))(0.3)(TeO(2))(0.7)]-xMnO, with x = 0.1, 0.2, 0.3 and 0.4 mol%, were successfully synthesized by using a conventional melt and quench-casting technique. In this study, the remelting effect of the glass samples on their microstructure was investigated through density measurement and FT-IR spectra and evaluated by XRD techniques. Initial experimental results from XRD evaluation show that there are two distinct phases of glassy and crystallite microstructure due to the existence of peaks in the sample. The different physical behaviors of the studied glasses were closely related to the concentration of manganese in each phase. FTIR spectra revealed that the addition of manganese oxide contributes the transformation of TeO(4) trigonal bipyramids with bridging oxygen (BO) to TeO(3) trigonal pyramids with non-bridging oxygen (NBO).
This study investigated the effect of annealing treatment (at 50°C for 72 h) on hydrolysis of tapioca and sweet potato starches using a raw starch hydrolyzing enzyme namely STARGEN 001 (a blend from fungal α-amylase and glucoamylase) at sub-gelatinization temperature (35°C) for 24 h. The degree of hydrolysis of the starches was evaluated based on the dextrose equivalent (DE) value. The hydrolyzed starches were then characterized in terms of its morphology, swelling power and solubility, gelatinization and pasting properties, amylose content and x-ray diffraction pattern. After 24 h of hydrolysis, annealed starches were hydrolyzed to a greater degree with higher DE value compared to native starches (40% vs 33% for tapioca; and 29% vs 24% for sweet potato starch). Scanning electron microscopy (SEM) micrographs revealed a more porous granules and rougher surface in annealed starches than their native counterparts. The swelling power and solubility of annealed starches decreased significantly. Annealing was found to affect the pasting properties of the starches appreciably and increase the starch gelatinization temperature. The amylose content in hydrolyzed annealed tapioca and sweet potato starches increased while no significant changes observed in the X-ray diffraction of those starches. This study shows that the annealing treatment can be used as a way to increase the degree of hydrolysis of tapioca and sweet potato starches at sub-gelatinization temperature using a raw starch hydrolyzing enzyme.
Production of carbon dioxide from degraded woods especially Karas or Aquilariella Malaccensis using integrated pyrolysis-combustion is important for radiocarbon dating application. The effects of pyrolysis temperatures (300-400 0 C), retention times (20-35 minutes) and flow rates of argon (400- 1000 ml/min) on the production of carbon dioxide were studied. The experiments were arranged according to a 2 3 response surface central composite statistical design (CSD). This response surface methodology (RSM) was used to assess factor interactions and empirical models regarding carbon dioxide yield. The optimized yield of carbon dioxide was 82.57% for Karas and the optimum reaction conditions are 300 0 C of pyrolysis temperature, 20 minutes retention time and 982ml/min flow rates of argon. Scanning electron microscope (SEM) and X-ray Diffraction (XRD) were conducted to assess the morphological characteristics of the woods and to look at the potential crystalline structure produced after the process took place, respectively.
The current research aimed at designing mesoporous silica nanoparticles (MSNs) for a controlled coadministration of salicylic acid (SA) and ketoconazole (KCZ) to effectively treat highly resistant fungal infections. The sol-gel method was used to formulate MSNs, which were further optimized using central composite rotatable design (CCRD) by investigating mathematical impact of independent formulation variables such as pH, stirring time, and stirring speed on dependent variables entrapment efficiency (EE) and drug release. The selected optimized MSNs and pure drugs were subjected to comparative in vitro/in vivo antifungal studies, skin irritation, cytotoxicity, and histopathological evaluations. The obtained negatively charged (-23.1), free flowing spherical, highly porous structured MSNs having a size distribution of 300-500 nm were suggestive of high storage stability and improved cell proliferation due to enhanced oxygen supply to cells. The physico-chemical evaluation of SA/KCZ-loaded MSNs performed through powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and thermal gravimetric analysis (TGA) indicates absolute lack of any interaction between formulation components and successful encapsulation of both drugs in MSNs. The EESA, EEKCZ, SA release, and KCZ release varied significantly from 34 to 89%, 36 to 85%, 39 to 88%, and 43 to 90%, respectively, indicating the quadratic impact of formulation variables on obtained MSNs. For MSNs, the skin tolerability and cell viability percentage rate were also having an extraordinary advantage over suspension of pure drugs. The optimized SA/KCZ-loaded MSNs demonstrated comparatively enhanced in vitro/in vivo antifungal activities and rapid wound healing efficacy in histopathological evaluation without any skin irritation impact, suggesting the MSNs potential for the simultaneous codelivery of antifungal and keratolyic agents in sustained release fashion.
Starch blend films made from sago and mung bean were prepared by casting with glycerol as the plasticizer and subsequently exposed to ultraviolet (UV) irradiation for 2 h. The films were characterized by thickness, moisture sorption isotherms, X-ray diffraction and Fourier transform infrared (FTIR) spectroscopy. All films produced were colorless while incorporation of glycerol resulted in more flexible and manageable films. Moisture sorption isotherms for all films showed sigmoidal shape and the control films showed slightly higher curve than treated films. While for X-ray analysis, the control and treated films for all formulations showed similar pattern, however for treated films showed more crystalline character. UV radiation showed affect on X-ray diffraction and sorption isotherms; however the UV radiation did not affect the spectra pattern of FTIR.
One-dimensional nanostructure materials are very attractive because of their electronic and optical properties depending on their size. It is well known that properties of material can be tuned by reducing size to nanoscale because at the small sizes, that they behave differently with its bulk materials and the band gap will control by the size. The tunability of the band gap makes nanostructured materials useful for many applications. As one of the wide band gaps semiconductor compounds, zinc selenide (ZnSe) nanostructures (nanoparticles, nanowires, nanorods) have received much attention for the application in optoelectronic devices, such as blue laser diode, light emitting diodes, solar cells and IR optical windows. In this study, ZnSe nanostructures have been synthesized by reduction process of zinc selenate using hydrazine hydrate (N2H4.2H2O). The reductive agent of hydrazine hydrate was added to the starting materials of zinc selenate were heat treated at 500 o C for 1 hour under argon flow to form onedimensional nanostructures. The SEM and TEM images show the formation of nanocompositelike structures, which some small nanobars and nanopellets stick to the rod. The x-ray diffraction and elemental composition analysis confirm the formation of mixture zinc oxide and zinc selenide phases.
In this study, a series of copper-ion-doped titanium dioxide (Cu-ion-doped TiO₂) nanotubes (NTs) were synthesized via a hydrothermal method by the concentration variation of doped Cu ions (0.00, 0.50, 1.00, 2.50, and 5.00 mmol). In addition, the samples were characterized using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), nitrogen gas adsorption measurements, and ultraviolet-visible (UV-Vis) diffuse-reflectance spectroscopy. The photocatalytic activity of the Cu-iondoped TiO₂ NTs was investigated for the degradation of methyl orange (MO) under sunlight. The results obtained from the structural and morphological studies revealed that, at low concentrations of Cu-doped TiO₂ NTs, Cu is incorporated into the interstitial positions of the TiO₂ lattice, affording a new phase of TiO₂ (hexagonal) instead of the anatase TiO₂ (tetragonal) observed for undoped TiO₂ NTs. EDX analysis confirmed the presence of Cu in the TiO₂-based photocatalyst. All of the investigated samples exhibited a hollow fibrous-like structure, indicative of an NT morphology. The inner and outer diameters of the NTs were 4 nm and 10 nm, respectively. The photocatalysts exhibited a large surface area due to the NT morphology and a type IV isotherm and H3 hysteresis, corresponding to the mesopores and slit-shaped pores. The Cu-ion-doped TiO₂ NTs were excited by sunlight because of their low bandgap energy; and after the incorporation of Cu ions into the interstitial positions of the TiO₂ lattice, the NTs exhibited high visible-light activity owing to the low bandgap.
A new organic-inorganic nanohybrid based on zinc-layered hydroxide intercalated with an anti-inflammatory agent was synthesized through direct reaction of salicylic acid at various concentrations with commercially available zinc oxide. The basal spacing of the pure phase nanohybrid was 15.73 Å, with the salicylate anions arranged in a monolayer form and an angle of 57 degrees between the zinc-layered hydroxide interlayers. Fourier transform infrared study further confirmed intercalation of salicylate into the interlayers of zinc-layered hydroxide. The loading of salicylate in the nanohybrid was estimated to be around 29.66%, and the nanohybrid exhibited the properties of a mesoporous-type material, with greatly enhanced thermal stability of the salicylate compared with its free counterpart. In vitro cytotoxicity assay revealed that free salicylic acid, pure zinc oxide, and the nanohybrid have a mild effect on viability of African green monkey kidney (Vero-3) cells.
In the present study, CMSS (carboxymethyl sago starch)-based hydrogel was synthesized by crosslinking with citric acid via esterification and then applied as a metal sorbent to overcome excessive heavy metal pollution. The CMSS/CA (carboxymethyl sago starch/citric acid) hydrogel was characterized by Fourier Transform Infrared (FT-IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). The absorption band at 1726 cm-1 was observed in the FT-IR spectrum of CMSS/CA hydrogel and indicated ester bonds formed. Further findings show that the cross-linkages in the CMSS/CA hydrogel increased the thermal stability of CMSS and various sizes of pores were also shown in the SEM micrograph. Conversely, the removal of heavy metals was analyzed using Inductively Coupled Plasma-Optic Emission Spectra (ICP-OES). The effects of the pH of the metal solution, contact time, initial concentration of the metal ions and temperature on the sorption capacity were investigated. Under optimum condition, the sorption capacity of Pb2+, Cu2+, Ni2+ and Zn2+ onto CMSS/CA hydrogel were 64.48, 36.56, 16.21, 18.45 mg/g, respectively. The experiments demonstrated that CMSS/CA hydrogel has high selectivity towards Pb2+ in both non-competitive and competitive conditions. In conclusion, the CMSS/CA hydrogel as a natural based heavy metal sorption material exhibited a promising performance, especially in the sorption of Pb2+ for wastewater treatment.
Recent environmental problems and societal concerns associated with the disposal of petroleum based plastics throughout the world have triggered renewed efforts to develop new biodegradable products compatible with our environment. This article describes the preparation, characterization and biodegradation study of poly(lactic acid)/layered double hydroxide (PLA/LDH) nanocomposites from PLA and stearate-Zn(3)Al LDH. A solution casting method was used to prepare PLA/stearate-Zn(3)Al LDH nanocomposites. The anionic clay Zn(3)Al LDH was firstly prepared by co-precipitation method from a nitrate salt solution at pH 7.0 and then modified by stearate anions through an ion exchange reaction. This modification increased the basal spacing of the synthetic clay from 8.83 Å to 40.10 Å. The morphology and properties of the prepared PLA/stearate-Zn(3)Al LDH nanocomposites were studied by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), thermogravimetric analysis (TGA), tensile tests as well as biodegradation studies. From the XRD analysis and TEM observation, the stearate-Zn(3)Al LDH lost its ordered stacking-structure and was greatly exfoliated in the PLA matrix. Tensile test results of PLA/stearate-Zn(3)Al LDH nanocomposites showed that the presence of around 1.0-3.0 wt % of the stearate-Zn(3)Al LDH in the PLA drastically improved its elongation at break. The biodegradation studies demonstrated a significant biodegradation rate improvement of PLA in the presence of stearate-Zn(3)Al LDH nanolayers. This effect can be caused by the catalytic role of the stearate groups in the biodegradation mechanism leading to much faster disintegration of nanocomposites than pure PLA.
Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.
The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks.
A metal-free mesoporous carbon nitride (MCN) was investigated for the first time as an adsorbent for N-nitrosopyrrolidine (NPYR), which is one of the nitrosamine pollutants. Under the same condition, the adsorption capability of the MCN was found to be higher than that of the MCM-41. Since the adsorption isotherm was consistent with Langmuir and Freundlich model equations, it was suggested that the adsorption of NPYR molecules on the MCN occurred in the form of mono-molecular layer on the heterogeneous surface sites. It was proposed that MCN with suitable adsorption sites was beneficial for the adsorption of NPYR. The evidence on the interaction between the NPYR molecules and the MCN was supported by fluorescence spectroscopy. Two excitation wavelengths owing to the terminal N-C and N=C groups were used to monitor the interactions between the emission sites of the MCN and the NPYR molecules. It was confirmed that the intensity of the emission sites was quenched almost linearly with the concentration of NPYR. This result obviously suggested that the MCN would be applicable as a fluorescence sensor for detection of the NPYR molecules. From the Stern-Volmer plot, the quenching rate constant of terminal N-C groups was determined to be ca. two times higher than that of the N=C groups on MCN, suggesting that the terminal N-C groups on MCN would be the favoured sites interacted with the NPYR. Since initial concentration can be easily recovered, the interactions of NPYR on MCN were weak and might only involve electrostatic interactions.
In this paper, densification of in-situ copper-niobium carbide composite using cold pressing technique was addressed. Mixtures of Cu-20vol%NbC powder were prepared by two methods.
In first method, a mixture of Cu-15.79wt%Nb-2.04wt%C powder was milled at 400 rpm for 35 hours in a planetary mill. In second method, Cu and commercial NbC powder was mixed at 100 rpm for 2 hours in a jar mill. Then, both powders were pressed at different pressure (i.e. 350 MPa, 450 MPa, 550 MPa and 650 MPa) and sintered at 900 o C for 1 hour. Sample of in-situ and ex-situ Cu-20vol%NbC composite were characterized for density, hardness, phase formation by x-ray diffraction analysis and microstructure by scanning electron microscope. Xray diffraction analysis showed that NbC phase was formed in the in-situ processed sample. Hardness of in-situ processed copper composite was higher than that of the ex-situ processed copper composite due to good interface between coper matrix and niobium carbide reinforcement particle as well as distribution of finer niobium carbide particles in copper matrix. Sintered density of in-situ composite is lower than density of ex-situ composite beacuse of work hardening of the Cu-Nb-C mixture powder during powder to ball collision. Density and hardness of the in-situ and ex-situ Cu-20vol%NbC composites increase with the increase in compaction pressure as porosity is eliminated at higher compaction pressure.
Hydroxyapatite is an ideal biomaterial for bone tissue engineering due to its biocompatibility and hemocompatibility which have been widely studied by many researchers. The incorporation of nanoporosity into hydroxyapatite could transform the biomaterial into an effective adsorbent for uremic toxins removal especially in artificial kidney system. However, the effect of nanoporosity incorporation on the hemocompatibility of hydroxyapatite has yet to be answered. In this study, nanoporous hydroxyapatite was synthesized using hydrothermal technique and its hemocompatibility was determined. Non-ionic surfactants were used as soft templates to create porosity in the hydroxyapatite. The presence of pure hydroxyapatite phase in the synthesized samples is validated by X-ray diffraction analysis and Fourier transform infrared spectroscopy. The TEM images show that the hydroxyapatite formed rod-like particles with the length of 21-90 nm and diameter of 11-70 nm. The hydroxyapatite samples exhibit BET surface area of 33-45 m2 g-1 and pore volume of 0.35-0.44 cm3 g-1. The hemocompatibility of the hydroxyapatite was determined via hemolysis test, platelet adhesion, platelet activation and blood clotting time measurement. The nanoporous hydroxyapatite shows less than 5% hemolysis, suggesting that the sample is highly hemocompatible. There is no activation and morphological change observed on the platelets adhered onto the hydroxyapatite. The blood clotting time demonstrates that the blood incubated with the hydroxyapatite did not coagulate. This study summarizes that the synthesized nanoporous hydroxyapatite is a highly hemocompatible biomaterial and could potentially be utilized in biomedical applications.
Zerumbone, a natural dietary lipophilic compound with low water solubility (1.296 mg/L at 25°C) was used in this investigation. The zerumbone was loaded into nanostructured lipid carriers using a hot, high-pressure homogenization technique. The physicochemical properties of the zerumbone-loaded nanostructured lipid carriers (ZER-NLC) were determined. The ZER-NLC particles had an average size of 52.68 ± 0.1 nm and a polydispersity index of 0.29 ± 0.004 μm. Transmission electron microscopy showed that the particles were spherical in shape. The zeta potential of the ZER-NLC was -25.03 ± 1.24 mV, entrapment efficiency was 99.03%, and drug loading was 7.92%. In vitro drug release of zerumbone from ZER-NLC was 46.7%, and for a pure zerumbone dispersion was 90.5% over 48 hours, following a zero equation. Using the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay in human T-cell acute lymphoblastic leukemia (Jurkat) cells, the half maximal inhibitory concentration (IC50) of ZER-NLC was 5.64 ± 0.38 μg/mL, and for free zerumbone was 5.39 ± 0.43 μg/mL after 72 hours of treatment. This study strongly suggests that ZER-NLC have potential as a sustained-release drug carrier system for the treatment of leukemia.