In this study, the unaffected, affected and heavily affected teeth were studied by using X-Ray diffraction method. The D-values, which are related to the crystallite size of the apatite crystals, were calculated according to the Sherrer equation. The crystallite size of unaffected enamel was found to be 1530.95Å, while the affected enamel was 1490.22Å and the heavily affected enamel was 1484.16Å respectively. This study showed that the unaffected enamel has greater crystallite size as compared to the affected and heavily affected enamel.
Piroxicam is a nonsteroidal anti-inflammatory drug with low aqueous solubility which exhibits polymorphism. The present study was carried out to develop polymorphs of piroxicam with enhanced solubility and dissolution rate by the crystal modification technique using different solvent mixtures prepared with PEG 4000 and PVP K30. Physicochemical characteristics of the modified crystal forms of piroxicam were investigated by X-ray powder diffractometry, FT-IR spectrophotometry and differential scanning calorimetry. Dissolution and solubility profiles of each modified crystal form were studied and compared with pure piroxicam. Solvent evaporation method (method I) produced both needle and cubic shaped crystals. Slow crystallization from ethanol with addition of PEG 4000 or PVP K30 at room temperature (method II) produced cubic crystal forms. Needle forms produced by method I improved dissolution but not solubility. Cubic crystals produced by method I had a dissolution profile similar to that of untreated piroxicam but showed better solubility than untreated piroxicam. Cubic shaped crystals produced by method II showed improved dissolution, without a significant change in solubility. Based on the XRPD results, modified piroxicam crystals obtained by method I from acetone/benzene were cube shaped, which correlates well with the FTIR spectrum; modified needle forms obtained from ethanol/methanol and ethanol/acetone showed a slight shift of FTIR peak that may be attributed to differences in the internal structure or conformation.
Band gap change in doped ZnO is an observed phenomenon that is very interesting from the fundamental point of view. This work is focused on the preparation of pure and single phase nanostructured ZnO and Cu as well as Mn-doped ZnO for the purpose of understanding the mechanisms of band gap narrowing in the materials. ZnO, Zn0.99Cu0.01O and Zn0.99Mn0.01O materials were prepared using a wet chemistry method, and X-ray diffraction (XRD) results showed that all samples were pure and single phase. UV-visible spectroscopy showed that materials in the nanostructured state exhibit band gap widening with respect to their micron state while for the doped compounds exhibited band gap narrowing both in the nano and micron states with respect to the pure ZnO materials. The degree of band gap change was dependent on the doped elements and crystallite size. X-ray photoelectron spectroscopy (XPS) revealed that there were shifts in the valence bands. From both UV-visible and XPS spectroscopy, it was found that the mechanism for band gap narrowing was due to the shifting of the valance band maximum and conduction band minimum of the materials. The mechanisms were different for different samples depending on the type of dopant and dimensional length scales of the crystallites.
Semiconductor thin films Copper Tin Selenide, Cu2SnSe3, a potential compound for solar cell applications or semiconductor radiation detector were prepared by thermal evaporation method onto well-cleaned glass substrates. The as-deposited films were annealed in flowing purified nitrogen N2, for 2 hours in a temperature range from 100˚C to 500˚C. The structure of as-deposited and annealed films has been studied by X-ray diffraction technique. The semi-quantitative analysis indicated from Reitveld refinement show that the samples composed of Cu2SnSe3 and SnSe. These studies revealed that the films were structured in mixed phase between cubic space group F-43m (no. 216) and orthorhombic space group P n m a (no. 62). The crystallite size and lattice strain were determined from Scherrer calculation method. The results show that increasing in annealing temperature resulted in direct increase in crystallite size and decrease in lattice strain.
This study was designed to investigate the crystallite sizes of Porites species. A set of 9 Porites skeletons i.e. Porites australiensis, Porites cylindrica, Porites lutea, Porites lichen, Porites digitata, Porites nigrescens, Porites rus, Porites annae and Porites sp. were studied by using XRay Diffraction method. The values of FWHM and theta (θ) are used in Scherrer equation to determine the crystallite sizes of all Porites samples. It was found that the crystallite sizes were in the range of 1007.78 Ǻ – 1706.04 Ǻ.
Ceramic of BaxSr1-xTiO3 (BST) for x =0.3; 0.5 and 0.7 were successfully deposited by solid solution method. The BST ceramic were analyzed by x-ray diffraction (XRD). The XRD spectra was recorded on a Philips type PW 3701 diffractometer using CuKD (Oco = 1.54056 Å) radiation at 30 KV and 30 mA (900 watt). The spectra shows that BST ceramic are polycrystalline with tetragonal structure. The lattice constants analysis of the grown ceramics was analyzed by visual basic program. Using Cohen’s and Cramer’s algorithms in visual basic program, , the lattice constants are a = b = 3.877 Å; c = 3.970 Å for Ba0.3Sr0.7TiO3 ceramic, a = b = 3.979 Å; c = 3.981 Å. for Ba0.5Sr0.5TiO3 ceramic and a = b = 3.965 Å; c = 4.005 Å for Ba0.7Sr0.3TiO3 ceramic, respectively. The reform value of the lattice constant of BST ceramic is possibly associated with the anti site defects of Ba and Sr.
Thermoplastic natural rubber sample is found isotropic based on SAXS pattern. Morphological parameter was obtained based on ideal lamellar morphology using 1-D correlation function. The fitting was carried out using Porod tail model and Vonk for back-extrapolated model. It is found that the long period value is 15.7nm which is comparable to results obtained from Lorents corrected profile, 20nm. Crystalline thickness and amorphous thickness was found as 13.4 and 2.31nm respectively
Microwave assisted wet precipitation method was used to synthesize calcium deficient strontium doped β-tricalcium phosphate (Sr-βTCP) with a chemical formula of Ca2.96-xSrx(PO4)2. Sr-βTCP was reacted with monocalcium phosphate monohydrate [Ca(H2PO4)2.H2O, MCPM] in presence of water to furnish corresponding Sr containing brushite cement (Sr-Brc). The samples were characterized by using X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM). Strontium content in the prepared samples was determined by using inductively coupled plasma optical emission spectrometry (ICP-OES). The effect of Sr2+ions on the structural, mechanical, setting properties and drug release of the cement is reported. Incorporation of Sr2+ions improved the injectability, setting time and mechanical properties of the Brc. The release profiles of antibiotics incorporated in Brc and Sr-Brc confirmed that the Sr incorporation into the Brc results in the efficient release of the antibiotics from the cement.
The structures of two new anthracenyl chalcones, namely (E)-1-(anthracen-9-yl)-3-(4-nitro-phen-yl)prop-2-en-1-one, C23H15NO3, and (E)-1-(anthracen-9-yl)-3-(4-iodo-phen-yl)prop-2-en-1-one, C23H15IO are reported. A structural comparative study between the two chalcones was performed and some effects on the geometrical parameters, such as planarity and dihedral angles, are described. The mol-ecular geometry was determined by single-crystal X-ray diffraction, and density functional theory (DFT) at B3LYP with the 6-311++G(d,p) basis set was applied to optimize the ground-state geometry. In addition, inter-molecular inter-actions responsible for the crystal packing were analysed. The electronic properties, such as excitation energies and HOMO-LUMO energies were calculated by time-dependent density functional theory (TD-DFT) and the results complement the experimental findings. The mol-ecular electrostatic potential (MEP) was also investigated at the same level of theory in order to identify and qu-antify the possible reactive sites.
We report the synthesis of amorphous carbon nanotubes/silver (αCNTs/Ag) nanohybrids via simple chemical route without additional reactant and surfactant at low temperature. Field emission scanning microscope (FESEM) and transmission electron microscope (TEM) confirmed formation of CNTs. X-ray diffraction (XRD) pattern confirmed the amorphous phase of carbon and the formation of Ag nanoparticles crystalline phase. Raman spectra revealed the amorphous nature of α CNTs. UV-visible spectroscopy showed enhancement of optical properties of α CNTs/Ag nanohybrids.
Synthetic branched-chain glycolipids are suitable as model systems in understanding biological cell membranes, particularly because certain natural lipids possess chain branching. Herein, four branched-chain glycopyranosides, namely, 2-hexyl-decyl-α-D-glucopyranoside (α-Glc-OC10C6), 2-hexyl-decyl-β-D-glucopyranoside (β-Glc-OC10C6), 2-hexyl-decyl-α-D-galactopyranoside (α-Gal-OC10C6), and 2-hexyl-decyl-β-D-galactopyranoside (β-Gal-OC10C6), with a total alkyl chain length of 16 carbon atoms have been synthesized, and their phase behavior has been studied. The partial binary phase diagrams of these nonionic surfactants in water were investigated by optical polarizing microscopy (OPM) and small-angle X-ray scattering (SAXS). The introduction of chain branching in the hydrocarbon chain region is shown to result in the formation of inverse structures such as inverse hexagonal and inverse bicontinuous cubic phases. A comparison of the four compounds showed that they exhibited different polymorphism, especially in the thermotropic state, as a result of contributions from anomeric and epimeric effects according to their stereochemistry. The neat α-Glc-OC10C6 compound exhibited a lamellar (Lα) phase whereas dry α-Gal-OC10C6 formed an inverse bicontinuous cubic Ia3d (QII(G)) phase. Both β-anomers of glucoside and galactoside adopted the inverse hexagonal phase (HII) in the dry state. Generally, in the presence of water, all four glycolipids formed inverse bicontinuous cubic Ia3d (QII(G)) and Pn3m (QII(D)) phases over wide temperature and concentration ranges. The formation of inverse nonlamellar phases by these Guerbet branched-chain glycosides confirms their potential as materials for novel biotechnological applications such as drug delivery and crystallization of membrane proteins.
The identification, characterization and quantification of crystal forms are becoming increasingly important within the pharmaceutical industry. A combination of different physical analytical techniques is usually necessary for this task. In this work solid-state techniques, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and X-ray powder diffractometry (XRPD) were combined to analyze polymorphic purity of crystalline ranitidine-HCl, an antiulcer drug, H2 receptor antagonists. A series of 12 different mixtures of Form 1 and 2 was prepared by geometric mixing and their DRIFT spectra and XRD powder patterns were obtained and analyzed, either alone or combined together, using Artificial Neural Networks (ANNs). A standard feed-forward network, with back-propagation rule and with multi layer perceptron architecture (MPL) was chosen. A working range of 1.0-100% (w/w) of crystal Form 2 in Form 1 was established with a minimum quantifiable level (MQL) of 5.2% and limit of detection of 1.5% (w/w). The results demonstrate that DRIFTS combined with XRPD may be successfully used to distinguish between the ranitidine-HCl polymorphs and to quantify the composition of binary mixtures of the two.
The in situ polymorphic forms and thermal transitions of refined, bleached and deodorized palm oil (RBDPO), palm stearin (RBDPS) and palm kernel oil (RBDPKO) were investigated using coupled X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicated that the DSC onset crystallisation temperature of RBDPO was at 22.6°C, with a single reflection at 4.2Å started to appear from 23.4 to 17.1°C, and were followed by two prominent exothermic peaks at 20.1°C and 8.5°C respectively. Further cooling to -40°C leads to the further formation of a β'polymorph. Upon heating, a of β'→βtransformation was observed between 32.1 to 40.8°C, before the sample was completely melted at 43.0°C. The crystallization onset temperature of RBDPS was 44.1°C, with the appearance of the α polymorph at the same temperature as the appearance of the first sharp DSC exothermic peak. This quickly changed from α→β´ in the range 25 to 21.7°C, along with the formation of a small β peak at -40°C. Upon heating, a small XRD peak for the β polymorph was observed between 32.2 to 36.0°C, becoming a mixture of (β´+ β) between 44.0 to 52.5°C. Only the β polymorph survived further heating to 59.8°C. For RBDPKO, the crystallization onset temperature was 11.6°C, with the formation of a single sharp exothermic peak at 6.5°C corresponding to the β' polymorphic form until the temperature reached -40°C. No transformation of the polymorphic form was observed during the melting process of RBDPKO, before being completely melted at 33.2°C. This work has demonstrated the detailed dynamics of polymorphic transformations of PKO and PS, two commercially important hardstocks used widely by industry and will contribute to a greater understanding of their crystallization and melting dynamics.
The release of chlorophenoxyherbicides agrochemicals, namely 2-chloro- (2CPA), 4-chloro and 2,4,5-trichloro (TCPA) phenoxyacetates from their nanohybrids into various aqueous solutions; carbonate, sulfate and chloride was found to be controlled by pseudo-second order rate expression. The percentage saturated released was found to be anionic-dependent, in the order of carbonate>sulfate>chloride for the release media and 2CPA>4CPA>TCPA for the anionic guests. This study demonstrates that the release of the phenoxyherbicides agrochemicals from the nanohybrid compounds can be tuned by choosing the right combination of exchangeable anions both the incoming and the outgoing anions.
The experiment aims to investigate the effect of high energy milling to the crystallite size of α-alumina. The starting material used is α-alumina powder with starting crystal size of 86nm. This powder was milled at different time ranges from 0 to 60 minutes and milling speed ranges from 400 rpm to 1100 rpm using a wet milling technique in corundum abrasive materials. The wet milling technique involved the use of water with the alumina to water ratio of 1:6.1. Samples prepared were then examined using the X-Ray Diffraction (XRD) to calculate the crystallite size and scanning electron microscope (SEM) was also used to determine changes in the morphology. Results from these analysis showed that the crystallite size will get smaller when milling speed and time of more than 600rpm and 30 minutes respectively were used. Optimum conditions to achieve the smallest crystal size of 79.7nm are 1000 rpm and 60 minutes.
Al/B4C composites with 0 wt.%, 5 wt.% and 10 wt.% of B4C were prepared by powder metallurgy and their properties were characterised successfully. Investigation of the effect of milling times (4, 8, 12, 16 hours) on microstructure, phase identification, hardness and neutron attenuation coefficient of composites has been studied. The results showed that hardness increased with increased of milling time, with maximum hardness obtained at 16 hours milling time. The increment is slower as the composition of B4C increased. The hardness of Al/10%B4C, Al/5%B4C and Al/0%B4C were 81.7, 78.7 and 61.2 HRB respectively. Morphology of scanning electron microscopy (SEM) showed that microstructures play important role in controlling the hardness. Meanwhile, x-ray diffraction (XRD) analysis showed the phases and crystalline present in composites with an indication that crystalline of the grain increased as the milling time increased. Neutron absorption of Al/10%B4C composites showed that this composite has the highest attenuation coefficient, thus indicating that it is the best composites for neutron shielding.
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
This research investigates and analyzes wear properties of 316 stainless steel before and after applying paste boronizing process and to investigate the effect of shot blasting process in enhancing boron dispersion into the steel. In order to enhance the boron dispersion into 316 stainless steel, surface deformation method by shot blasting process was deployed. Boronizing treatment was conducted using paste medium for 8 hours under two different temperatures which were 8500 C and 9500 C. Wear behaviour was evaluated using pin-on-disc test for abrasion properties. The analysis on microstructure, X-ray Diffraction (XRD) and density were also carried out before and after applying boronizing treatment. Boronizing process that had been carried out on 316 stainless steel increases the wear resistance of the steel compared to the unboronized 316 stainless steel. The effect of boronizing treatment together with the shot blasting process give a greater impact in increasing the wear resistance of 316 stainless steel. This is mainly because shot blasted samples initiated surface deformation that helped more boron dispersion due to dislocation of atom on the deformed surface. Increasing the boronizing temperature also increases the wear resistance of 316 stainless steel. In industrial application, the usage of the components that have been fabricated using the improved 316 stainless steel can be maximized because repair and replacement of the components can be reduced as a result of improved wear resistance of the 316 stainless steel.
Ca0.5Sr0.5Cu3Ti4O12 (CSCTO) ceramic oxide was prepared using solid state reaction technique. Impedance measurement was done using High Dielectric Resolution Analyzer (Novocontrol Novotherm) from 30 oC to 250 oC, in the frequency range of 10-2 to 106 Hz. X-ray diffraction pattern showed a single phase with a cubic structure. In the complex impedance plot, three semi-circles were observed; these represented the grain, grain boundary and electrode effect responses. The semi-circles were fitted using a series network of three parallel RC circuits. The resistance was found to increase with the decreasing temperature. The activation energies, Ea, obtained from the Arrhenius plots of CSCTO, were 0.31 eV and 0.73 eV for grain and grain boundary conductivity, respectively. The value of the grain energy was revealed as smaller than the grain boundary energy, due to the semi-conducting grain and the insulating grain boundary characteristic (Sinclair et al., 2002).
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.