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Powder Diffractometry (powder + diffractometry)
Kinds of Powder Diffractometry Selected AbstractsSynthesis, Crystal Structure Determination from X-Ray Powder Diffractometry and Vibrational Spectroscopic Properties of Mg[N(CN)2]2×4H2O.CHEMINFORM, Issue 36 2005Elisabeth Irran Abstract For Abstract see ChemInform Abstract in Full Text. [source] Synthesis of rhombohedral strontium carbonate aggregates at the water/hexamethylene interface with cetyltrimethylammonium bromideCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2008Long Chen Abstract Unusual rhombohedral strontium carbonate (SrCO3) aggregates have been synthesized in situ from strontium nitrate by the slow release of carbon dioxide by alkaline hydrolysis of diethyl carbonate at the water/hexamethylene interface in the presence of cetyltrimethylammonium bromide (CTAB). Transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray powder diffractometry were used to characterize the products. The results indicate that rhombohedral SrCO3 aggregates are obtained with weaker crystallinity and sizes of several micrometers. The possible formation mechanism of the SrCO3 aggregates at the interface is discussed, which can be interpreted by particle-aggregation based non-classical crystallization laws. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Influence of the starting powders on the synthesis of nickel ferriteCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2006F. Kenfack Abstract The thermal decomposition of freeze-dried nickel(II)-iron(III) formate was investigated by means of DTA, TG, mass spectrometry and X-ray powder diffractometry. For the preparation of homogeneous freeze-dried nickel(II)-iron(III) formate precursors, a rigorous control of nickel ion concentration in the precursor solution was required. The decomposition of the reactive nickel(II)-iron(III) formate does not only reflect aspects of single formates, but also an interaction between components which lowers the decomposition temperature. Crystalline nickel ferrite powders were obtained at 600-800°C. This temperature is quite lower than 1100°C employed for the ceramic method. In the presence of air, the regeneration of nickel ferrite from the taenite phase (,Ni,Fe) is accomplished at 800°C. This temperature is also 300°C below the temperature employed when the mixtures NiO:,-Fe2O3 or Ni:2Fe are the starting powders. The main reason for the high reactivity of the freeze-dried formates and the taenite alloy is the large homogeneity of these precursors. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Physicochemical characterization and antioxidant activity of quercetin-loaded chitosan nanoparticlesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2008Yuying Zhang Abstract Quercetin is an abundant flavonoid in food plants with numerous biological activities and widely used as a potent antioxidant. Being sparingly soluble in water and subject to degradation in aqueous intestinal fluids, the absorption of quercetin is limited upon oral administration. In the present study, chitosan nanoparticles and quercetin-loaded nanoparticles were prepared based on the ionic gelation of chitosan with tripolyphosphate anions. The encapsulation of quercetin in the chitosan nanoparticles were confirmed by differential scanning calorimetry, X-ray powder diffractometry, Fourier transformed infrared spectroscopy, ultraviolet-visible spectrum, and fluorescence spectrum. The morphology of the nanoparticles was characterized by atomic force microscopy. The antioxidant activity of the quercetin-nanoparticles was also evaluated in vitro by two different methods (free radical scavenging activity test and reducing power test), which indicates that inclusion of quercetin in chitosan nanopaticles may be useful in improving the bioavailabilty of quercetin. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008 [source] Unexpected fluorescence emission of poly(,,,- L -malic acid) in aqueous mediumJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Yaofeng Fan Abstract Unexpected fluorescence of poly(,,,- L -malic acid) (,,,-PMA) without traditional fluorophore was observed firstly. This fluorescent polymer was synthesized via melt polycondensation of L -malic acid. The polymer was characterized by gel permeation chromatography (GPC), nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), thermogravimetry (TG), Fourier transform infrared spectroscopy (IR), Fourier transform Raman spectroscopy (Raman), and X-ray powder diffractometry (XRD). The high molecular weight ,,,-PMA was synthesized by the optimum polycondensation at 130°C for 15 h, followed by fractional precipitation with diethyl ether and petroleum ether. The degree of branching of ,,,-PMA was from 10% to 20% according to the reaction condition. Terminal group of ,,,-PMA was mainly hydroxycarboxylic group companied with a few CHCHCOOH groups owing to dehydration of a normal terminal during the melt polycondensation. A fluorescence emission maximum of ,,,-PMA in water appeared at 420 nm when it was excited at 340 nm. Further study indicated that the fluorescence intensity was concentration-dependent, pH-dependent, and molecular-weight-dependent. The fluorescence formation may result from multichain aggregations, which was formed readily in aqueous solution due to intermolecular hydrogen bonds between branched ,,,-PMA. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007 [source] Characterization and use of acid-activated montmorillonite-illite type of clay for lead(II) removalAICHE JOURNAL, Issue 9 2010John U. Kennedy Oubagaranadin Abstract The natural local deposits of montmorillonite-illite type of clay (MIC) were susceptible for acid activation. Raw clay was taken for experimentation, disintegrated on acid activation with sulfuric acid, which showed a particle size distribution. The montmorillonite and illite phases in the raw clay disappeared on acid activation and the activated clay, MIC(AA), showed with sodium-aluminum-silicate and beidellite phases apart from quartz (low) phase. The raw and acid-activated clays were characterized using X-ray powder diffractometry, X-ray fluorescence, Fourier transform infrared spectrometry, and energy dispersive X-ray, and their adsorption capacities were compared. When tested for adsorption of Pb(II) in aqueous solutions, the acid-activated clay showed about 50% increased adsorption than raw clay. Sips adsorption isotherm and pseudo-second-order kinetic models were found to be best for the batch adsorption data. Kinetic studies showed the existence of film diffusion and intraparticle diffusion. A two-stage batch adsorber was designed for the removal of Pb(II) from aqueous solutions. © 2010 American Institute of Chemical Engineers AIChE J, 2010 [source] Differences in the interaction between aryl propionic acid derivatives and poly(vinylpyrrolidone) K30: A multi-methodological approachJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 11 2009Zehadin Gashi Abstract The present work aims at the application of several methods to explain differences in the physical interaction of some aryl propionic acid derivatives (ibuprofen [IBP], ketoprofen [KET], flurbiprofen [FLU], naproxen [NAP], fenbufen [FEN]) with poly(vinylpyrrolidone) (PVP) K30, stored together at 298,±,0.5 K and 22% RH. X-ray powder diffractometry and 13C-solid state NMR demonstrated that IBP was able to strongly interact with the polymer, while weak interaction was observed for KET, FLU, NAP, and the least for FEN. The interaction of comelted drug and PVP was studied by differential scanning calorimetry by applying the Gordon,Taylor equation, which revealed that small molar drug volumes may favour the drug diffusion through the PVP amorphous chains increasing the polymer free volume and decreasing the mixture Tg. The molecular docking study revealed that intermolecular energy is mainly due to the contribution of van der Waals energy component, causing the differences among the drugs, and is related to the drug,PVP surface contact area in the complex formed. Solid-state kinetic study demonstrated that IBP molecules are involved in a three-dimensional diffusion mechanism within the polymer favoured by its low molar volume that reduces molecular hindrance, and by the weakness of its crystal lattice, which facilitates crystallinity loss and stabilisation of the amorphous phase. © 2009 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 98:4216,4228, 2009 [source] The effect of bulking agents on the chemical stability of acid-sensitive compounds in freeze-dried formulations: Sucrose inversion studyJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 9 2009Enxian Lu Abstract The goal of the study was to evaluate the impact of amorphous bulking agents on the chemical stability of freeze-dried materials. Polyvinylpyrrolidone and dextran of different molecular weights and lactose were used as bulking agents, and sucrose was used as an example of an acid-sensitive compound. Lyophiles containing bulking agent and sucrose at 10:1 (w/w) ratio, citrate buffer, and optionally bromophenol blue (pH indicator) were tested by X-ray powder diffractometry, differential scanning calorimetry, and Karl Fischer titrimetry. Diffuse reflectance UV,vis spectroscopy was used to obtain the concentration ratio of the deprotonated (In2,) to the protonated (HIn,) indicator species, from which the Hammett acidity function (H2,) was calculated. The extent of sucrose inversion in lyophiles stored at 60°C was quantified by HPLC. The bulking agent had a major impact on both the apparent solid-state acidity (H2,) and the degradation rate, with the degradation rate constants value highest for dextran lyophiles (most "acidic", lower H2,) followed by lactose and polyvinylpyrrolidone lyophile (least "acidic", higher H2,). The Hammett acidity function can be used as an empirical solid-state acidity scale, to predict the rank-order stability of acid-sensitive compounds in lyophiles prepared with different bulking agents. © 2009 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 98:3387,3396, 2009 [source] Establishing quantitative in-line analysis of multiple solid-state transformations during dehydrationJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 11 2008Karin Kogermann Abstract The aim of the study was to conduct quantitative solid phase analysis of piroxicam (PRX) and carbamazepine (CBZ) during isothermal dehydration in situ, and additionally exploit the constructed quantitative models to analyze the solid-state forms in-line during fluidized bed drying. Vibrational spectroscopy (near-infrared (NIR), Raman) was employed for monitoring the dehydration and the quantitative model was based on partial least squares (PLS) regression. PLS quantification was confirmed experimentally using isothermal thermogravimetric analysis (TGA) and X-ray powder diffractometry (XRPD). To appraise the quality of quantitative models several model parameters were evaluated. The hot-stage spectroscopy quantification results were found to be in reasonable agreement with TGA and XRPD results. Quantification of PRX forms showed complementary results with both spectroscopic techniques. The solid-state forms observed during CBZ dihydrate dehydration were quantified with Raman spectroscopy, but NIR spectroscopy failed to differentiate between the anhydrous solid-state forms of CBZ. In addition to in situ dehydration quantification, Raman spectroscopy in combination with PLS regression enabled in-line analysis of the solid-state transformations of CBZ during dehydration in a fluidized bed dryer. © 2008 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 97:4983,4999, 2008 [source] Phase transformation of erythromycin A dihydrate during fluid bed dryingJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 9 2008Meike Römer Abstract An in-line near infrared (NIR) spectrometer was employed to monitor phase transformations of erythromycin dihydrate during a miniaturized fluid bed drying process. The pellets, containing 50% (w/w) erythromycin dihydrate and 50% (w/w) microcrystalline cellulose, were dried at 30, 45, and 60°C. Principal component analysis was used to determine solid-state changes. For this purpose the wavelength range of 1360,2000 nm was selected and preprocessed to remove multiplicative effects. Transformation to erythromycin dehydrate was observed for the pellets dried at 45 and 60°C by NIR spectrometry and X-ray powder diffractometry (XRPD). The formation of erythromycin dehydrate was observed at a moisture content 1.4% (w/w) (mass of water per dry mass of sample) while at 1.8% (w/w) neither XRPD nor NIR were able to detect dehydration. Transformation to erythromycin dehydrate therefore depends strongly on the moisture content of the pellets. © 2007 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 97:4020,4029, 2008 [source] Characterization and crystal structure of D -mannitol hemihydrateJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 11 2004Cletus Nunes Abstract The objectives of this study were (i) to isolate and characterize mannitol hydrate, and (ii) to solve its crystal structure from high-resolution synchrotron X-ray powder diffraction data. Mannitol hydrate was prepared by freeze-drying aqueous mannitol solutions (5% w/v) under controlled conditions. X-ray powder diffractometry, differential scanning calorimetry, and thermogravimetric analyses indicated that mannitol exists as a hemihydrate (C6H14O6,·,0.5H2O). Synchrotron data were collected on the X3B1 beamline at the National Synchrotron Light Source. The simulated annealing program PSSP was used to solve the structure, which was subsequently refined by Rietveld analysis using the program package GSAS. The compound crystallizes in space group P1, with a,=,9.8963 Å, b,=,10.5424 Å, c,=,4.7860 Å, ,,=,102.589°, ,,=,86.092°, and ,,=,116.079°. The unit cell contains two dissimilar D -mannitol molecules and one water molecule, forming a hydrogen bonding pattern significantly different from that seen in the anhydrous polymorphs. © 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:2800,2809, 2004 [source] Solute crystallization in mannitol,glycine systems,implications on protein stabilization in freeze-dried formulationsJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 11 2003Abira Pyne Abstract The use of mannitol in combination with glycine has resulted in stable freeze-dried protein formulations. Our objectives were to (1) study solute crystallization in ternary systems containing mannitol, glycine, and water during all the stages of freeze drying as a function of processing conditions and formulation variables; (2) investigate the effect of sodium phosphate buffer salts on the crystallization of both mannitol and glycine and vice versa; and (3) investigate the effects of these excipients in a freeze-dried lactate dehydrogenase (LDH) formulation. X-ray powder diffractometry (XRD) and differential scanning calorimetry (DSC) were used to study the frozen aqueous solutions. Phase transitions during primary and secondary drying were monitored by simulating the entire freeze-drying process in situ in the sample chamber of the diffractometer. LDH activity after freeze drying was determined spectrophotometrically. In frozen aqueous solutions containing mannitol and glycine, each solute influenced the extent of crystallization of the other. The solutes crystallized as ,-mannitol and ,-glycine during primary drying. Glycine had a stronger tendency to crystallize, while it was easier to influence mannitol crystallization. The buffer salts inhibited the crystallization of mannitol and glycine. However, in some cases, during primary drying, glycine crystallization was followed by that of disodium hydrogen phosphate dodecahydrate. The latter underwent dehydration forming an amorphous anhydrate. It was possible to correlate the extent of crystallization of mannitol and glycine in the lyophile with the retention of protein activity. An increase in buffer concentration decreased the crystallinity of mannitol and glycine. This translated to increased retention of protein activity. © 2003 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 92:2272,2283, 2003 [source] Polymorphism of racemic felodipine and the unusual series of solid solutions in the binary system of its enantiomersJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 7 2001Judith M. Rollinger Abstract The aim of this study was to investigate the binary phase diagram and the polymorphism and pseudopolymorphism of racemic and enantiomeric felodipine, including their spectroscopic and thermodynamic properties. Different crystal forms were obtained by crystallization from solvents or from the annealed melt and investigated by thermal analysis (hot stage microscopy, differential scanning calorimetry, thermogravimetric analysis), spectroscopic methods (Fourier transform infrared,and Fourier transform,Raman spectroscopy), and X-ray powder diffractometry. The binary melting phase diagram was constructed based on thermoanalytical investigations of quantitative mixtures of (+)- and (±)-felodipine. Two polymorphic forms of racemic felodipine, mod. I (mp, ,145°C) and mod. II (mp, ,135°C), as well as an acetone solvate (SAc,) were characterized. Melting equilibria of felodipine crystal forms decrease due to thermal decomposition. Enantiomeric felodipine was found to be dimorphic (En-mod. I: mp, ,144°C; En-mod. II: mp, ,133°C). Evaluation of the binary system of (+)- and (,)-felodipine results in the formation of a continuous series of mixed crystals between the thermodynamically stable and higher melting modifications, mod. I and En-mod. I. Their unusual curve course, termed as Roozeboom Type 2 b, passes through a maximum in the racemic mixture and is flanked by a minimum at 20% and at 80% (+)-felodipine. From the thermodynamic parameters, racemic mod. I and II are monotropically related. In contrast to SAc, the thermodynamically unstable mod. II shows a considerable kinetic stability. Because its crystallization is badly reproducible, the use of mod. II is not advisable for processing. However, desolvation of SAc leads to a profitable crystal shape of mod. I, representing a pseudoracemate by definition. © 2001 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 90:949,959, 2001 [source] | ||||||||||