Scholarly Research Excellence

Digital Open Science Index

Commenced in January 2007 Frequency: Monthly Edition: International Paper Count: 27

Effect of Si/Al Ratio on SSZ-13 Crystallization and Its Methanol-To-Olefins Catalytic Properties

SSZ-13 materials with different Si/Al ratio were prepared by varying the composition of aluminosilicate precursor solutions upon hydrothermal treatment at 150 °C. The Si/Al ratio of the initial system was systematically changed from 12.5 to infinity in order to study the limits of Al composition in precursor solutions for constructing CHA structure. The intermediates and final products were investigated by complementary techniques such as XRD, HRTEM, FESEM, and chemical analysis. NH3-TPD was used to study the Brønsted acidity of SSZ-13 samples with different Si/Al ratios. The effect of the Si/Al ratio on the precursor species, ultimate crystal size, morphology and yield was investigated. The results revealed that Al species determine the nucleation rate and the number of nuclei, which is tied to the morphology and yield of SSZ-13. The size of SSZ-13 increased and the yield decreased as the Si/Al ratio was improved. Varying Si/Al ratio of the initial system is a facile, commercially viable method of tailoring SSZ-13 crystal size and morphology. Furthermore, SSZ-13 materials with different Si/Al ratio were tested as catalysts for the methanol to olefins (MTO) reaction at 350 °C. SSZ-13 with the Si/Al ratio of 35 shows the best MTO catalytic performance.

Ultrasound Assisted Cooling Crystallization of Lactose Monohydrate

α-lactose monohydrate is widely used in the pharmaceutical industries as an inactive substance that acts as a vehicle or a medium for a drug or other active substance. It is a byproduct of dairy industries, and the recovery of lactose from whey not only boosts the improvement of the economics of whey utilization but also causes a reduction in pollution as lactose recovery can reduce the BOD of whey by more than 80%. In the present study, levels of process parameters were kept as initial lactose concentration (30-50% w/w), sonication amplitude (20-40%), sonication time (2-6 hours), and crystallization temperature (10-20 oC) for the recovery of lactose in ultrasound assisted cooling crystallization. In comparison with cooling crystallization, the use of ultrasound enhanced the lactose recovery by 39.17% (w/w). The parameters were optimized for the lactose recovery using Taguchi Method. The optimum conditions found were initial lactose concentration at level 3 (50% w/w), amplitude of sonication at level 2 (40%), the sonication time at level 3 (6 hours), and crystallization temperature at level 1 (10 °C). The maximum recovery was found to be 85.85% at the optimum conditions. Sonication time and the initial lactose concentration were found to be significant parameters for the lactose recovery.

Experimental Investigation on Freeze-Concentration Process Desalting for Highly Saline Brines

Using the freeze-melting process for the disposing of high saline brines was the aim of the paper by confirming the performance estimation of the treatment system. A laboratory bench scale freezing technique test unit was designed, constructed, and tested at Doha Research Plant (DRP) in Kuwait. The principal unit operations that have been considered for the laboratory study are: ice crystallization, separation, washing, and melting. The applied process is characterized as “the secondary-refrigerant indirect freezing”, which is utilizing normal freezing concept. The high saline brine was used as definite feed water, i.e. average TDS of 250,000 ppm. Kuwait desalination plants were carried out in the experimental study to measure the performance of the proposed treatment system. Experimental analysis shows that the freeze-melting process is capable of dropping the TDS of the feed water from 249,482 ppm to 56,880 ppm of the freeze-melting process in the two-phase’s course, whereas overall recovery results of the salt passage and salt rejection are 31.11%, 19.05%, and 80.95%, correspondingly. Therefore, the freeze-melting process is encouraging for the proposed application, as it shows on the results, which approves the process capability of reducing a major amount of the dissolved salts of the high saline brine with reasonable sensible recovery. This process might be reasonable with other brine disposal processes.

Degradation of Irradiated UO2 Fuel Thermal Conductivity Calculated by FRAPCON Model Due to Porosity Evolution at High Burn-Up

The evolution of volume porosity previously obtained by using the existing low temperature high burn-up gaseous swelling model with progressive recrystallization for UO2 fuel is utilized to study the degradation of irradiated UO2 thermal conductivity calculated by the FRAPCON model of thermal conductivity. A porosity correction factor is developed based on the assumption that the fuel morphology is a three-phase type, consisting of the as-fabricated pores and pores due to intergranular bubbles whitin UO2 matrix and solid fission products. The predicted thermal conductivity demonstrates an additional degradation of 27% due to porosity formation at burn-up levels around 120 MWd/kgU which would cause an increase in the fuel temperature accordingly. Results of the calculations are compared with available data.

The Use of Secondary Crystallization in Cement-Based Composites
The paper focuses on the study of the properties of cement-based composites produced using secondary crystallization (crystalline additive). In this study, cement mortar made with secondary crystallization was exposed to an aggressive environment and the influence of secondary crystallization on the degradation of the cementitious composite was investigated. The results indicate that the crystalline additive contributed to increasing the resistance of the cement-based composite to the attack of the selected environments (sodium sulphate solution and ammonium chloride solution).
Extraction of Squalene from Lebanese Olive Oil

Squalene is a valuable component of the oil composed of 30 carbon atoms and is mainly used for cosmetic materials. The main concern of this article is to study the Squalene composition in the Lebanese olive oil and to compare it with foreign oil results. To our knowledge, extraction of Squalene from the Lebanese olive oil has not been conducted before. Three different techniques were studied and experiments were performed on three brands of olive oil, Al Wadi Al Akhdar, Virgo Bio and Boulos. The techniques performed are the Fractional Crystallization, the Soxhlet and the Esterification. By comparing the results, it is found that the Lebanese oil contains squalene and Soxhlet method is the most effective between the three methods extracting about 6.5E-04 grams of Squalene per grams of olive oil.

Studying the Intercalation of Low Density Polyethylene/Clay Nanocomposites after Different UV Exposures
This study attempts to understand the effect of different UV irradiation methods on the intercalation of LDPE/MMT nanocomposites, and its molecular behavior at certain isothermal crystallization temperature. Three different methods of UV exposure were employed using single composition of LDPE/MMT nanocomposites. All samples were annealed for 5 hours at a crystallization temperature of 100oC. The crystallization temperature was chosen to be at large supercooling temperature to ensure quick and complete crystallization. The raw material of LDPE consisted of two stable monoclinic and orthorhombic phases according to XRD results. The thermal behavior of both phases acted differently when UV exposure method was changed. The monoclinic phase was more dependent on the method used compared to the orthorhombic phase. The intercalation of clay, as well as, the non-isothermal crystallization temperature, has also shown a clear dependency on the type of UV exposure. A third phase that is thermally less stable was also observed. Its respond to UV irradiation was greater since it contains low molecular weight entities which make it more vulnerable to any UV exposure.
Determination of Recrystallization Temperature of Varying Degrees Formed Aluminium, by DMTA Technique
This study is about the structural transformations of aluminium examining with the Dynamic Mechanical Thermal Analyzer (DMTA). It is a faster and simpler measuring method to make consequence about the metal’s structural transformations. The device measures the changing of the mechanical characteristics depending on the heating rate, and concludes certain transformations. This measuring method fast and shows clean-cut results comparing the conventional ways. Applying polymer measuring devices for metal investigations is not widespread method. One of the adaptable ways is shown in this study. The article compares the results of the small specimen test and the DMTA method, considering the temperature and the forming dependence of recrystallization temperature.
Effect of Humidity on in-Process Crystallization of Lactose during Spray Drying

The effect of various humidities on process yields and degrees of crystallinity for spray-dried powders from spray drying of lactose with humid air in a straight-through system have been studied. It has been suggested by Williams–Landel–Ferry kinetics (WLF) that a higher particle temperature and lower glass-transition temperature would increase the crystallization rate of the particles during the spray-drying process. Freshly humidified air produced by a Buchi-B290 spray dryer as a humidifier attached to the main spray dryer decreased the particle glass-transition temperature (Tg), while allowing the particle temperature (Tp) to reach higher values by using an insulated drying chamber. Differential scanning calorimetry (DSC) and moisture sorption analysis were used to measure the degree of crystallinity for the spray-dried lactose powders. The results showed that higher Tp-Tg, as a result of applying humid air, improved the process yield from 21 ± 4 to 26 ± 2% and crystallinity of the particles by decreasing the latent heat of crystallization from 43 ± 1 to 30 ± 11 J/g and the sorption peak height from 7.3 ± 0.7% to 6 ± 0.7%.

The Experimental Measurement of the LiBr Concentration of a Solar Absorption Machine

The excessive consumption of fossil energies (electrical energy) during summer caused by the technological development involves more and more climate warming.

In order to reduce the worst impact of gas emissions produced from classical air conditioning, heat driven solar absorption chiller is pretty promising; it consists on using solar as motive energy which is clean and environmentally friendly to provide cold.

Solar absorption machine is composed by four components using Lithium Bromide /water as a refrigerating couple. LiBr- water is the most promising in chiller applications due to high safety, high volatility ratio, high affinity, high stability and its high latent heat. The lithium bromide solution is constitute by the salt lithium bromide which absorbs water under certain conditions of pressure and temperature however if the concentration of the solution is high in the absorption chillers; which exceed 70%, the solution will crystallize.

The main aim of this article is to study the phenomena of the crystallization and to evaluate how the dependence between the electric conductivity and the concentration which should be controlled.

Structural and Computational Studies of N-[(2,6-Diethylphenyl) carbamothioyl]-2,2-diphenylacetamide, N-[(3 Ethylphenyl) carbamothioyl]-2,2-diphenylacetamide and 2,2-Diphenyl-N-{[2-(trifluoromethyl) phenyl]carbamothioyl}acetamide

Theoretical investigations are performed by DFT method of B3LYP/6-31G+(2d,p) and B3LYP/6-311G+(2d,p) basis sets for three carbonyl thiourea compounds, namely N-[(2,6-Diethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound I), N-[(3-Ethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound II) and 2,2-Diphenyl-N-{[2-(trifluoromethyl)phenyl]carbamothioyl}acetamide (Compound III). Theoretical calculations for bond parameters, harmonic vibration frequencies and isotropic chemical shifts are in good agreement with the experimental results. The calculated molecular vibrations show good correlation values, which are 0.998 and 0.999 with the experimental data. The energy gap for compounds I, II and III calculated at B3LYP/6-31G+(2d,p) basis set are 4.455866117, 4.297495791 and 4.313550514 eV respectively, while for B3LYP/6-311G+(2d,p) basis set the energy gap obtained are 4.453689205 (Compound I), 4.311373603 (Compound II) and 4.315727426 (Compound III) eV.

Carbon Dioxide Recovery by Membrane Assisted Crystallization

This study addresses the effect of impurities on the crystallization of Na2CO3 produced within a strategy for capturing CO2 from flue gases by alkaline absorption. A novel technology - membrane assisted crystallization - is proposed for Na2CO3 crystallization from mother liquors containing impurities. High purity of Na2CO3•10H2O crystals was obtained without impacting the performance of the mass transfer of water vapor through membranes during crystallization.

Evaluation and Preparation of Crystal Modifications of Artesunate: In vivo Studies

Five crystal modifications of water insoluble artesunate were generated by recrystallizing it from various solvents with improved physicochemical properties. These generated crystal forms were characterized to select the most potent and soluble form. SEM of all the forms showed changes in external shape leading them to be different morphologically. DSC thermograms of Form III and Form V showed broad endotherm peaks at 83.04oC and 76.96oC prior to melting fusion of drug respectively. Calculated weight loss in TGA revealed that Form III and Form V are methanol and acetone solvates respectively. However, few additional peaks were appeared in XRPD pattern in these two solvate forms. All forms exhibit exothermic behavior in buffer and two solvates display maximum ease of molecular release from the lattice. Methanol and acetone solvates were found to be most soluble forms and exhibited higher antimalarial efficacy showing higher survival rate (83.3%) after 30 days.

High Temperature Deformation Behavior of Cr-containing Superplastic Iron Aluminide
Superplastic deformation and high temperature load relaxation behavior of coarse-grained iron aluminides with the composition of Fe-28 at.% Al have been investigated. A series of load relaxation and tensile tests were conducted at temperatures ranging from 600 to 850oC. The flow curves obtained from load relaxation tests were found to have a sigmoidal shape and to exhibit stress vs. strain rate data in a very wide strain rate range from 10-7/s to 10-2/s. Tensile tests have been conducted at various initial strain rates ranging from 3×10-5/s to 1×10-2/s. Maximum elongation of ~500 % was obtained at the initial strain rate of 3×10-5/s and the maximum strain rate sensitivity was found to be 0.68 at 850oC in binary Fe-28Al alloy. Microstructure observation through the optical microscopy (OM) and the electron back-scattered diffraction (EBSD) technique has been carried out on the deformed specimens and it has revealed the evidences for grain boundary migration and grain refinement to occur during superplastic deformation, suggesting the dynamic recrystallization mechanism. The addition of Cr by the amount of 5 at.% appeared to deteriorate the superplasticity of the binary iron aluminide. By applying the internal variable theory of structural superplasticity, the addition of Cr has been revealed to lower the contribution of the frictional resistance to dislocation glide during high temperature deformation of the Fe3Al alloy.
Static Recrystallization Behavior of Mg Alloy Single Crystals
Single crystals of Magnesium alloys such as pure Mg, Mg-1Zn-0.5Y, Mg-0.1Y, and Mg-0.1Ce alloys were successfully fabricated in this study by employing the modified Bridgman method. To determine the exact orientation of crystals, pole figure measurement using X-ray diffraction were carried out on each single crystal. Hardness and compression tests were conducted followed by subsequent recrysatllization annealing. Recrystallization kinetics of Mg alloy single crystals has been investigated. Fabricated single crystals were cut into rectangular shaped specimen and solution treated at 400oC for 24 hrs, and then deformed in compression mode by 30% reduction. Annealing treatment for recrystallization has been conducted on these cold-rolled plates at temperatures of 300oC for various times from 1 to 20 mins. The microstructure observation and hardness measurement conducted on the recrystallized specimens revealed that static recrystallization of ternary alloy single crystal was very slow, while recrystallization behavior of binary alloy single crystals appeared to be very fast.
Characterization of Biodegradable Nanocomposites with Poly (Lactic Acid) and Multi-Walled Carbon Nanotubes
In this study, structural, mechanical, thermal and electrical properties of poly (lactic acid) (PLA) nanocomposites with low-loaded (0-1.5 wt%) untreated, heat and nitric acid treated multiwalled carbon nanotubes (MWCNTs) were studied. Among the composites, untreated 0.5 wt % MWCNTs and acid-treated 1.0 wt% MWCNTs reinforced PLA show the tensile strength and modulus values higher than the others. These two samples along with pure PLA exhibit the stable orthorhombic α-form, whilst other samples reveal the less stable orthorhombic β-form, as demonstrated by X-ray diffraction study. Differential scanning calorimetry reveals the evolution of the mentioned different phases by controlled cooling and discloses an enhancement of PLA crystallization by nanotubes incorporation. Thermogravimetric analysis shows that the MWCNTs loaded sample degraded faster than PLA. Surface resistivity of the nanocomposites is found to be dropped drastically by a factor of 1013 with a low loading of MWCNTs (1.5 wt%).
The removal of Ni, Cu and Fe from a Mixed Metal System using Sodium Hypophosphite as a Reducing Agent

The main objective of this study was to remove and recover Ni, Cu and Fe from a mixed metal system using sodium hypophosphite as a reducing agent and nickel powder as seeding material. The metal systems studied consisted of Ni-Cu, Ni-Fe and Ni-Cu-Fe solutions. A 5 L batch reactor was used to conduct experiments where 100 mg/l of each respective metal was used. It was found that the metals were reduced to their elemental form with removal efficiencies of over 80%. The removal efficiency decreased in the order Fe>Ni>Cu. The metal powder obtained contained between 97-99% Ni and was almost spherical and porous. Size enlargement by aggregation was the dominant particulate process.

Non-Isothermal Kinetics of Crystallization and Phase Transformation of SiO2-Al2O3-P2O5-CaO-CaF Glass
The crystallization kinetics and phase transformation of SiO2.Al2O3.0,56P2O5.1,8CaO.0,56CaF2 glass have been investigated using differential thermal analysis (DTA), x-ray diffraction (XRD), and scanning electron microscopy (SEM). Glass samples were obtained by melting the glass mixture at 14500С/120 min. in platinum crucibles. The mixture were prepared from chemically pure reagents: SiO2, Al(OH)3, H3PO4, CaCO3 and CaF2. The non-isothermal kinetics of crystallization was studied by applying the DTA measurements carried out at various heating rates. The activation energies of crystallization and viscous flow were measured as 348,4 kJ.mol–1 and 479,7 kJ.mol–1 respectively. Value of Avrami parameter n ≈ 3 correspond to a three dimensional of crystal growth mechanism. The major crystalline phase determined by XRD analysis was fluorapatite (Ca(PO4)3F) and as the minor phases – fluormargarite (CaAl2(Al2SiO2)10F2) and vitlokite (Ca9P6O24). The resulting glass-ceramic has a homogeneous microstructure, composed of prismatic crystals, evenly distributed in glass phase.
Effects of FAU Zeolites on the Crystallization of Chloronitrobenzenes above the Eutectic Composition
Crystallization has been used for the separation of chloronitrobenzene or CNBs, which are isomeric substances (o-, mand p-CNB) and important intermediates in chemical productions. Effects of feed composition on the crystallization of m- and p-CNB was first studied. The results conform to the binary phase diagram of m- and p-CNB. After that, effects of FAU zeolites (NaX, CaX, BaX, NaY and CaY) above the eutectic composition (63.5 and 65.0 wt% m-CNB in the feed) was also investigated. The results showed that the FAU zeolites significantly affected the precipitates, the composition of which was shifted from being rich in m-CNB to rich in p-CNB. Effects of the number of FAU zeolites on the precipitate composition was then studied. The results revealed that the precipitates from the lower number of the zeolites had higher p-CNB purity than those from the higher number of zeolite.
An Automated High Pressure Differential Thermal Analysis System for Phase Transformation Studies
A piston cylinder based high pressure differential thermal analyzer system is developed to investigate phase transformations, melting, glass transitions, crystallization behavior of inorganic materials, glassy systems etc., at ambient to 4 GPa and at room temperature to 1073 K. The pressure is calibrated by the phase transition of bismuth and ytterbium and temperature is calibrated by using thermocouple data chart. The system developed is calibrated using benzoic acid, ammonium nitrate and it has a pressure and temperature control of ± 8.9 x 10 -4 GPa , ± 2 K respectively. The phase transition of Asx Te100-x chalcogenides, ferrous oxide and strontium boride are studied using the indigenously developed system.
Effect of CW Laser Annealing on Silicon Surface for Application of Power Device
As application of re-activation of backside on power device Insulated Gate Bipolar Transistor (IGBT), laser annealing was employed to irradiate amorphous silicon substrate, and resistivities were measured using four point probe measurement. For annealing the amorphous silicon two lasers were used at wavelength of visible green (532 nm) together with Infrared (793 nm). While the green laser efficiently increased temperature at top surface the Infrared laser reached more deep inside and was effective for melting the top surface. A finite element method was employed to evaluate time dependent thermal distribution in silicon substrate.
X-ray Crystallographic Analysis of MinC N-Terminal Domain from Escherichia coli
MinC plays an important role in bacterial cell division system by inhibiting FtsZ assembly. However, the molecular mechanism of the action is poorly understood. E. coli MinC Nterminus domain was purified and crystallized using 1.4 M sodium citrate pH 6.5 as a precipitant. X-ray diffraction data was collected and processed to 2.3 Å from a native crystal. The crystal belonged to space group P212121, with the unit cell parameters a = 52.7, b = 54.0, c = 64.7 Å. Assuming the presence of two molecules in the asymmetric unit, the Matthews coefficient value is 1.94 Å3 Da-1, which corresponds to a solvent content of 36.5%. The overall structure of MinCN is observed as a dimer form through anti-parallel ß-strand interaction.
Geochemistry of Cenozoic Basaltic Rocksaround Liuhe National Geopark, Jiangsu Province, Eastern China: Petrogenesis and Mantle Source
Cenozoic basalts found in Jiangsu province of eastern China include tholeiites and alkali basalts. The present paper analyzed the major, trace elements, rare earth elements of these Cenozoic basalts and combined with Sr-Nd isotopic compositions proposed by Chen et al. (1990)[1] in the literatures to discuss the petrogenesis of these basalts and the geochemical characteristics of the source mantle. Based on major, trace elements and fractional crystallization model established by Brooks and Nielsen (1982)[2] we suggest that the basaltic magma has experienced olivine + clinopyroxene fractionation during its evolution. The chemical compositions of basaltic rocks from Jiangsu province indicate that these basalts may belong to the same magmatic system. Spidergrams reveal that Cenozoic basalts from Jiangsu province have geochemical characteristics similar to those of ocean island basalts(OIB). The slight positive Nb and Ti anomalies found in basaltic rocks of this study suggest the presence of Ti-bearing minerals in the mantle source and these Ti-bearing minerals had contributed to basaltic magma during partial melting, indicating a metasomatic event might have occurred before the partial melting. Based on the Sr vs. Nd isotopic ratio plots, we suggest that Jiangsu basalts may be derived from partial melting of mantle source which may represent two-end members mixing of DMM and EM-I. Some Jiangsu basaltic magma may be derived from partial melting of EM-I heated by the upwelling asthenospheric mantle or asthenospheric diapirism.
EBSD Investigation of Friction Stir Welded Duplex Stainless Steel

Electron back-scattered diffraction was used to follow the evolution of microstructure from the base metal to the stir zone (SZ) in a duplex stainless steel subjected to friction stir welding. In the stir zone (SZ), a continuous dynamic recrystallization (CDRX) was evidenced for ferrite, while it was suggested that a static recrystallization together with CDRX may occur for austenite. It was found that ferrite and austenite grains in the SZ take a typical shear texture of bcc and fcc materials respectively.

Model based Soft-Sensor for Industrial Crystallization: On-line Mass of Crystals and Solubility Measurement
Monitoring and control of cane sugar crystallization processes depend on the stability of the supersaturation (σ ) state. The most widely used information to represent σ is the electrical conductivity κ of the solutions. Nevertheless, previous studies point out the shortcomings of this approach: κ may be regarded as inappropriate to guarantee an accurate estimation of σ in impure solutions. To improve the process control efficiency, additional information is necessary. The mass of crystals in the solution ( c m ) and the solubility (mass ratio of sugar to water / s w m m ) are relevant to complete information. Indeed, c m inherently contains information about the mass balance and / s w m m contains information about the supersaturation state of the solution. The main problem is that c m and / s w m m are not available on-line. In this paper, a model based soft-sensor is presented for a final crystallization stage (C sugar). Simulation results obtained on industrial data show the reliability of this approach, c m and the crystal content ( cc ) being estimated with a sufficient accuracy for achieving on-line monitoring in industry
Neural Network-Based Control Strategies Applied to a Fed-Batch Crystallization Process
This paper is focused on issues of process modeling and two model based control strategies of a fed-batch sugar crystallization process applying the concept of artificial neural networks (ANNs). The control objective is to force the operation into following optimal supersaturation trajectory. It is achieved by manipulating the feed flow rate of sugar liquor/syrup, considered as the control input. The control task is rather challenging due to the strong nonlinearity of the process dynamics and variations in the crystallization kinetics. Two control alternatives are considered – model predictive control (MPC) and feedback linearizing control (FLC). Adequate ANN process models are first built as part of the controller structures. MPC algorithm outperforms the FLC approach with respect to satisfactory reference tracking and smooth control action. However, the MPC is computationally much more involved since it requires an online numerical optimization, while for the FLC an analytical control solution was determined.
Application of Feed Forward Neural Networks in Modeling and Control of a Fed-Batch Crystallization Process

This paper is focused on issues of nonlinear dynamic process modeling and model-based predictive control of a fed-batch sugar crystallization process applying the concept of artificial neural networks as computational tools. The control objective is to force the operation into following optimal supersaturation trajectory. It is achieved by manipulating the feed flow rate of sugar liquor/syrup, considered as the control input. A feed forward neural network (FFNN) model of the process is first built as part of the controller structure to predict the process response over a specified (prediction) horizon. The predictions are supplied to an optimization procedure to determine the values of the control action over a specified (control) horizon that minimizes a predefined performance index. The control task is rather challenging due to the strong nonlinearity of the process dynamics and variations in the crystallization kinetics. However, the simulation results demonstrated smooth behavior of the control actions and satisfactory reference tracking.

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