Abstract: In this study, the transesterification of palm oil with methanol for biodiesel production was studied by using CaO–ZnO as a heterogeneous base catalyst prepared by incipient-wetness impregnation (IWI) and co-precipitation (CP) methods. The reaction parameters considered were molar ratio of methanol to oil, amount of catalyst, reaction temperature, and reaction time. The optimum conditions–15:1 molar ratio of methanol to oil, a catalyst amount of 6 wt%, reaction temperature of 60 °C, and reaction time of 8 h–were observed. The effects of Ca loading, calcination temperature, and catalyst preparation on the catalytic performance were studied. The fresh and spent catalysts were characterized by several techniques, including XRD, TPR, and XRF.
Abstract: In this study, Li4SiO4 powder was successfully
synthesized via sol gel method followed by drying at 150oC. Lithium
oxide, Li2O and silicon oxide, SiO2 were used as the starting
materials with citric acid as the chelating agent. The obtained powder
was then sintered at various temperatures. Crystallographic phase
analysis, morphology and ionic conductivity were investigated
systematically employing X-ray diffraction, Fourier Transform
Infrared, Scanning Electron Microscopy and AC impedance
spectroscopy. XRD result showed the formation of pure monoclinic
Li4SiO4 crystal structure with lattice parameters a = 5.140 Å, b =
6.094 Å, c = 5.293 Å, β = 90o in the sample sintered at 750oC. This
observation was confirmed by FTIR analysis. The bulk conductivity
of this sample at room temperature was 3.35 × 10-6 S cm-1 and the
highest bulk conductivity of 1.16 × 10-4 S cm-1 was obtained at
100°C. The results indicated that, the Li4SiO4 compound has
potential to be used as host for LISICON structured solid electrolyte
for low temperature application.
Abstract: The photocatalytic activity efficiency of TiO2 for the degradation of Toluene in photoreactor can be enhanced by nano- TiO2/LDPE composite film. Since the amount of TiO2 affected the efficiency of the photocatalytic activity, this work was mainly concentrated on the effort to embed the high amount of TiO2 in the Polyethylene matrix. The developed photocatalyst was characterized by XRD, UV-Vis spectrophotometer and SEM. The SEM images revealed the high homogeneity of the deposition of TiO2 on the polyethylene matrix. The XRD patterns interpreted that TiO2 embedded in the PE matrix exhibited mainly in anatase form. In addition, the photocatalytic results show that the toluene removal efficiencies of 30±5%, 49±4%, 68±5%, 42±6% and 33±5% were obtained when using the catalyst loading at 0%, 10%, 15%, 25% and 50% (wt. cat./wt. film), respectively.
Abstract: This study investigated a strategy of blending lead-laden sludge and Al-rich precursors to reduce the release of metals from the stabilized products. Using PbO as the simulated lead-laden sludge to sinter with γ-Al2O3 by Pb:Al molar ratios of 1:2 and 1:12, PbAl2O4 and PbAl12O19 were formed as final products during the sintering process, respectively. By firing the PbO + γ-Al2O3 mixtures with different Pb/Al molar ratios at 600 to 1000 °C, the lead transformation was determined through X-ray diffraction (XRD) data. In Pb/Al molar ratio of 1/2 system, the formation of PbAl2O4 is initiated at 700 °C, but an effective formation was observed above 750 °C. An intermediate phase, Pb9Al8O21, was detected in the temperature range of 800-900 °C. However, different incorporation behavior for sintering PbO with Al-rich precursors at a Pb/Al molar ratio of 1/12 was observed during the formation of PbAl12O19 in this system. In the sintering process, both temperature and time effect on the formation of PbAl2O4 and PbAl12O19 phases were estimated. Finally, a prolonged leaching test modified from the U.S. Environmental Protection Agency-s toxicity characteristic leaching procedure (TCLP) was used to evaluate the durability of PbO, Pb9Al8O21, PbAl2O4 and PbAl12O19 phases. Comparison for the leaching results of the four phases demonstrated the higher intrinsic resistance of PbAl12O19 against acid attack.
Abstract: In the present study Schwertmannite (an iron oxide
hydroxide) is selected as an adsorbent for defluoridation of water.
The adsorbent was prepared by wet chemical process and was
characterized by SEM, XRD and BET. The fluoride adsorption
efficiency of the prepared adsorbent was determined with respect to
contact time, initial fluoride concentration, adsorbent dose and pH of
the solution. The batch adsorption data revealed that the fluoride
adsorption efficiency was highly influenced by the studied factors.
Equilibrium was attained within one hour of contact time indicating
fast kinetics and the adsorption data followed pseudo second order
kinetic model. Equilibrium isotherm data fitted to both Langmuir and
Freundlich isotherm models for a concentration range of 5-30 mg/L.
The adsorption system followed Langmuir isotherm model with
maximum adsorption capacity of 11.3 mg/g. The high adsorption
capacity of Schwertmannite points towards the potential of this
adsorbent for fluoride removal from aqueous medium.
Abstract: The mesoporous MoO3/γ-Al2O3 catalyst was prepared
by incipient wetness impregnation method aiming to investigate the
effect of drying method and molybdenum content on the catalyst
property and performance towards the oxidation of benzothiophene
(BT), dibenzothiophene (DBT) and 4,6-dimethyle dibenzothiophene
(4,6-DMDBT) with H2O2 for deep oxidative desulfurization of diesel
fuel. The catalyst was characterized by XRD, BET, BJH and SEM
method. The catalyst with 10wt.% and 15wt.% Mo content represent
same optimum performance for DBT and 4,6-DMDBT removal, but
a catalyst with 10wt.% Mo has higher efficiency than 15wt.% Mo for
BT conversion. The SEM images show that use of rotary evaporator
in drying step reaches a more homogenous impregnation. The
oxidation reactivity of different sulfur compounds was studied which
followed the order of DBT>4,6-DMDBT>>BT.
Abstract: In this study, synthesis of biomemitic patterned nano
hydroxyapatite-starch biocomposites using different concentration of
starch to evaluate effect of polymer alteration on biocomposites
structural properties has been reported. Formation of hydroxyapatite
nano particles was confirmed by X-ray diffraction (XRD) and Fourier
transform infrared spectroscopy (FT-IR). Size and morphology of the
samples were characterized using scanning and transmission electron
microscopy (SEM and TEM). It seems that by increasing starch
content, the more active site of polymer (oxygen atoms) can be
provided for interaction with Ca2+ followed by phosphate and
hydroxyl group.
Abstract: Electrochemical-oxidation of Reactive Black-5 (RB- 5) was conducted for degradation using DSA type Ti/RuO2-SnO2- Sb2O5 electrode. In the study, for electro-oxidation, electrode was indigenously fabricated in laboratory using titanium as substrate. This substrate was coated using different metal oxides RuO2, Sb2O5 and SnO2 by thermal decomposition method. Laboratory scale batch reactor was used for degradation and decolorization studies at pH 2, 7 and 11. Current density (50mA/cm2) and distance between electrodes (8mm) were kept constant for all experiments. Under identical conditions, removal of color, COD and TOC at initial pH 2 was 99.40%, 55% and 37% respectively for initial concentration of 100 mg/L RB-5. Surface morphology and composition of the fabricated electrode coatings were characterized using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) respectively. Coating microstructure was analyzed by X-ray diffraction (XRD). Results of this study further revealed that almost 90% of oxidation occurred within 5-10 minutes.
Abstract: Nano sized zirconium dioxide in monoclinic phase (m-ZrO2) has been synthesized in pure form through co-precipitation processing at different calcination temperatures and has been characterized by several techniques such as XRD, FT-IR, UV-Vis Spectroscopy and SEM. The dielectric and capacitance values of the pelletized samples have been examined at room temperature as the functions of frequency. The higher dielectric constant value of the sample having larger grain size proves the strong influence of grain size on the dielectric constant.
Abstract: Fly ash is one of the residues generated in
combustion, and comprises the fine particles that rise with the flue
gases. Ash which does not rise is termed bottom ash [1]. In our
country, it is expected that will be occurred 50 million tons of waste
ash per year until 2020. Released waste from the thermal power
plants is caused very significant problems as known. The fly ashes
can be evaluated by using as adsorbent material.
The purpose of this study is to investigate the possibility of use of
Tuncbilek fly ash like low-cost adsorbents for heavy metal
adsorption. First of all, Tuncbilek fly ash was characterized. For this
purpose; analysis such as sieve analysis, XRD, XRF, SEM and FT-IR
were performed.
Abstract: A simple and dexterous in situ method was introduced to load CdS nanocrystals into organofunctionalized mesoporous, which used an ion-exchange method. The products were extensively characterized by combined spectroscopic methods. X- ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) demonstrated both the maintenance of pore symmetry (space group p6mm) of SBA-15 and the presence of CdS nanocrystals with uniform sizes of about 6 - 8 nm inside the functionalized SBA-15 channels. These mesoporous silica-supported CdS composites showed room temperature photoluminescence properties with a blue shift, indicating the quantum size effect of nanocrystalline CdS.
Abstract: The mineral having chemical compositional formula MgAl2O4 is called “spinel". The ferrites crystallize in spinel structure are known as spinel-ferrites or ferro-spinels. The spinel structure has a fcc cage of oxygen ions and the metallic cations are distributed among tetrahedral (A) and octahedral (B) interstitial voids (sites). The X-ray diffraction (XRD) intensity of each Bragg plane is sensitive to the distribution of cations in the interstitial voids of the spinel lattice. This leads to the method of determination of distribution of cations in the spinel oxides through XRD intensity analysis. The computer program for XRD intensity analysis has been developed in C language and also tested for the real experimental situation by synthesizing the spinel ferrite materials Mg0.6Zn0.4AlxFe2- xO4 and characterized them by X-ray diffractometry. The compositions of Mg0.6Zn0.4AlxFe2-xO4(x = 0.0 to 0.6) ferrites have been prepared by ceramic method and powder X-ray diffraction patterns were recorded. Thus, the authenticity of the program is checked by comparing the theoretically calculated data using computer simulation with the experimental ones. Further, the deduced cation distributions were used to fit the magnetization data using Localized canting of spins approach to explain the “recovery" of collinear spin structure due to Al3+ - substitution in Mg-Zn ferrites which is the case if A-site magnetic dilution and non-collinear spin structure. Since the distribution of cations in the spinel ferrites plays a very important role with regard to their electrical and magnetic properties, it is essential to determine the cation distribution in spinel lattice.
Abstract: There are many kinds of metal borates found not only
in nature but also synthesized in the laboratory such as magnesium
borates. Due to its excellent properties, as remarkable ceramic
materials, they have also application areas in anti-wear and friction
reducing additives as well as electro-conductive treating agents. The
synthesis of magnesium borate powders can be fulfilled simply with
two different methods, hydrothermal and thermal synthesis.
Microwave assisted method, also another way of producing
magnesium borate, can be classified into thermal synthesis because of
using the principles of solid state synthesis. It also contributes
producing particles with small size and high purity in nano-size
material synthesize. In this study the production of magnesium
borates, are aimed using MgCl2.6H2O and H3BO3. The identification
of both starting materials and products were made by the equipments
of, X-Ray Diffraction (XRD) and Fourier Transform Infrared
Spectroscopy (FT-IR). After several synthesis steps magnesium
borates were synthesized and characterized by XRD and FT-IR, as
well.
Abstract: Batch adsorption of recalcitrant melanoidin using the abundantly available coal fly ash was carried out. It had low specific surface area (SBET) of 1.7287 m2/g and pore volume of 0.002245 cm3/g while qualitative evaluation of the predominant phases in it was done by XRD analysis. Colour removal efficiency was found to be dependent on various factors studied. Maximum colour removal was achieved around pH 6, whereas increasing sorbent mass from 10g/L to 200 g/L enhanced colour reduction from 25% to 86% at 298 K. Spontaneity of the process was suggested by negative Gibbs free energy while positive values for enthalpy change showed endothermic nature of the process. Non-linear optimization of error functions resulted in Freundlich and Redlich-Peterson isotherms describing sorption equilibrium data best. The coal fly ash had maximum sorption capacity of 53 mg/g and could thus be used as a low cost adsorbent in melanoidin removal.
Abstract: Turkey has 72 % of total world boron reserves on the
basis of B2O3.Borates that is a refined form of boron minerals have a
wide range of applications. Zinc borates can be used as multifunctional
synergistic additives. The most important properties are
low solubility in water and high dehydration temperature. Zinc
borates dehydrate above 290°C and anhydrous zinc borate has
thermal resistance about 400°C. Zinc borates can be synthesized
using several methods such as hydrothermal and solid-state
processes. In this study, the solid-state method was applied between
500 and 800°C using the starting materials of ZnO and H3BO3 with
1:4 mole ratio. The reaction time was determined as 4 hours after
some preliminary experiments. After the synthesis, the crystal
structure and the morphology of the products were examined by XRay
Diffraction (XRD), Fourier Transform Infrared Spectroscopy
(FT-IR) and Raman Spectrometer. As a result the form of ZnB4O7
was synthesized with the highest crystal score at 800°C.
Abstract: Hydrothermally synthesized high silica borosilicates
with the MFI structure was subjected to several characterization
techniques. The effect of boron on the structure and acidity of
HZSM-5 catalyst were studied by XRD, SEM, N2 adsorption, solid
state NMR, NH3-TPD. It was confirmed that boron had entered the
framework in the boron samples. The results also revealed that strong
acidity was weakened and weak acidity was strengthened by the
boron added zeolite framework compared with parent catalyst. The
catalytic performance was carried out in a fixed bed at 460°C for
methanol to propylene (MTP) reaction. The results of MTP reaction
showed a great increment of the propylene selectivity and excellent
stability for the B-HZSM-5. The catalyst exhibited about 81%
selectivity to C2
= - C4
= olefins with 40% selectivity of propylene as
major component at near 100% methanol conversion, and the stable
performance in the studied period was 100h.
Abstract: The nickel and gold nanoclusters as supported
catalysts were analyzed by XAS, XRD and XPS in order to
determine their local, global and electronic structure. The present
study has pointed out a strong deformation of the local structure of
the metal, due to its interaction with oxide supports. The average
particle size, the mean squares of the microstrain, the particle size
distribution and microstrain functions of the supported Ni and Au
catalysts were determined by XRD method using Generalized Fermi
Function for the X-ray line profiles approximation. Based on EXAFS
analysis we consider that the local structure of the investigated
systems is strongly distorted concerning the atomic number pairs.
Metal-support interaction is confirmed by the shape changes of the
probability densities of electron transitions: Ni K edge (1s →
continuum and 2p), Au LIII-edge (2p3/2 → continuum, 6s, 6d5/2 and
6d3/2). XPS investigations confirm the metal-support interaction at
their interface.
Abstract: In the present work homogeneous silica film on
silicon was fabricated by colloidal silica sol. The silica sol precursor
with uniformly granular particle was derived by the alkaline
hydrolysis of tetraethoxyorthosilicate (TEOS) in presence of glycerol
template. The film was prepared by dip coating process. The
templated hetero-structured silica film was annealed at elevated
temperatures to generate nano- and meso porosity in the film. The
film was subsequently annealed at different temperatures to make it
defect free and abrasion resistant. The sol and the film were
characterized by the measurement of particle size distribution,
scanning electron microscopy, XRD, FTIR spectroscopy,
transmission electron microscopy, atomic force microscopy,
measurement of the refractive index, thermal conductivity and
abrasion resistance. The porosity of the films decreased whereas
refractive index and dielectric constant of it `increased with the
increase in the annealing temperature. The thermal conductivity of
the films increased with the increase in the film thickness. The
developed porous silica film holds strong potential for use in
different areas.
Abstract: An ecofriendly Citrus paradisipeel extract mediated synthesis of TiO2 nanoparticles is reported under sonication. U.V.-vis, Transmission electron microscopy, Dynamic light scattering, and X-ray analyses are performed to characterize the formation of TiO2 nanoparticles. It is almost spherical in shape, having a size of 60–140 nm and the XRD peaks at 2θ = 25.363° confirm the characteristic facets for anatase form. The synthesized nanocatalyst is highly active in the decomposition of methyl orange (64 mg/L) in sunlight (~73%) for 2.5h.
Abstract: Powder of La0.6Sr0.4CoO3-α (LSCO) was synthesized
by a combined citrate-EDTA method. The as-synthesized LSCO
powder was calcined, respectively at temperatures of 800, 900 and
1000 °C with different heating/cooling rates which are 2, 5, 10 and
15 °C min-1. The effects of heat treatments on the phase formation of
perovskite phase of LSCO were investigated by powder X-ray
diffraction (XRD). The XRD patterns revealed that the rate of
5 °C min-1 is the optimum heating/cooling rate to obtain a single
perovskite phase of LSCO with calcination temperature of 800 °C.
This result was confirmed by a thermogravimetric analysis (TGA) as
it showed a complete decomposition of intermediate compounds to
form oxide material was also observed at 800 °C.