Home About us Contact
|
Home About us Contact | ||
|
|
||
Crystalline Sample (crystalline + sample)
Selected AbstractsGrowth and properties of ferroelectric potassium ferrocyanide trihydrate single crystalsCRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2006R. Kanagadurai Abstract Single crystals of potassium ferrocyanide trihydrate, K4[Fe(CN)6·3H2O (KFCT), a ferroelectric material with Curie temperature 251K were grown in silica gel at room temperature for the first time by the solubility reduction method. Resorcinol and ethyl alcohol were used for the purpose of gel setting and supernatant liquid respectively. Optical and mechanical properties were studied for the grown crystal. The structure of the grown crystal was confirmed by X-ray diffraction analysis. Fourier Transform Infrared (FTIR) and FT Raman spectral analysis of the crystalline samples reveal that the crystalline sample consist consists of all functional groups. Thermal analysis of the crystalline sample was performed by TGA and DTA methods. The Vicker's micro hardness value was measured for KFCT crystals. The square etch pits with a hopper-like structure is an indicative of 2D nucleation mechanism. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Rare-Earth Spontaneous Emission Control in Three-Dimensional Lithium Niobate Photonic CrystalsADVANCED MATERIALS, Issue 34 2009Airán Ródenas Spontaneous emission inhibition of erbium ions at 1.5,µm wavelength is obtained by tailoring direct femtosecond-laser-written 3D photonic structures inside lithium niobate laser crystals. This technique allows for engineering of the structure symmetry and filling fraction by spatially inscribing laser-induced amorphous voxels inside the crystalline sample. [source] Photocatalytic Selective Oxidation of 4-Methoxybenzyl Alcohol to Aldehyde in Aqueous Suspension of Home-Prepared Titanium Dioxide CatalystADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 6 2007Giovanni Palmisano Abstract The photocatalytic oxidation of 4-methoxybenzyl alcohol to p -anisaldehyde (PAA) was performed in water with organic-free suspensions of home-prepared and commercial titanium dioxide (TiO2) catalysts. The nanostructured TiO2 samples were synthesised by boiling aqueous solutions of titanium tetrachloride (TiCl4), under mild conditions, for different times. The crystallinity increased with the boiling time. The 4-methoxybenzyl alcohol oxidation rate followed the same pattern but the highest yield (41.5,% mol) to PAA was found for the least crystalline sample, that showed a quantum efficiency of 0.116,%. A comparison with two commercial TiO2 samples showed that all the home-prepared catalysts exhibited a PAA yield higher than that of commercial ones. The only by-products present were traces of 4-methoxybenzoic acid and aliphatic products, carbon dioxide being the other main oxidation product. [source] The Structure of Yttrialite and Its Identification Using Laboratory and Synchrotron-Based Powder X-Ray DiffractionJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2009William J. Heward A highly crystalline sample of the impurity stabilized phase y -Y2Si2O7, generally known as yttrialite, has been formed from the melt of a glass with a nominal composition of 62(SiO2),10(Al2O3),28(Y2O3) mol%. Powder X-ray diffraction patterns were collected using in-house instrumentation and the 11-BM diffractometer at the Advanced Photon Source, Argonne National Laboratory, Argonne, IL. Rietveld refinements were carried out on the patterns using two structural models. On patterns collected using in-house instrumentation the correct structure assignment was difficult to determine; however, the extremely high-quality data afforded by the 11-BM instrument showed conclusively that the sample was found to crystallize in the monoclinic system (SG=P21/m) with lattice parameters a=5.03032(6), b=8.06892(6), c=7.33620(6) Ĺ, and ,=108.673(1). Furthermore, simulations have shown that it is likely that this structure model can be used to describe natural yttrialite or yttrialite that is formed at low temperatures, though the possibility that such materials are paracrystalline is also discussed. [source] X-ray and 13C solid-state NMR studies of N -benzoyl-phenylalanineCHEMICAL BIOLOGY & DRUG DESIGN, Issue 4 2000M.J. Potrzebowski Abstract: A crystalline sample of N -benzoyl- dl -phenylalanine 1 and a polycrystalline sample of N -benzoyl- l -phenylalanine 2 were studied using 13C high-resolution solid-state NMR spectroscopy. The X-ray structure of the dl form was established. Sample 1 crystallizes in a monoclinic form with a P21/c space group, a = 11.338(1) Ĺ, b = 9.185(1) Ĺ, c = 14.096(2) Ĺ, ,,= 107.53(3)°, V = 1400(3) Ĺ3, Z = 4 and R = 0.053. The principal elements of the 13C chemical shift tensors ,ii for 1 and 2, selectively 13C (99%) labeled at the carboxyl groups were calculated. On the basis of 13C ,ii analysis the hydrogen bonding pattern for sample 2 was deduced. Enriched samples were used to establish the intermolecular distance between chemically equivalent nuclei for 1 and spatial proximity in heterogeneous domain for 2, employing the ODESSA pulse sequence. The consistence of the complementary approach covering X-ray data, analysis of the 13C ,ii parameters and ODESSA results is revealed. [source] Growth and properties of ferroelectric potassium ferrocyanide trihydrate single crystalsCRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2006R. Kanagadurai Abstract Single crystals of potassium ferrocyanide trihydrate, K4[Fe(CN)6·3H2O (KFCT), a ferroelectric material with Curie temperature 251K were grown in silica gel at room temperature for the first time by the solubility reduction method. Resorcinol and ethyl alcohol were used for the purpose of gel setting and supernatant liquid respectively. Optical and mechanical properties were studied for the grown crystal. The structure of the grown crystal was confirmed by X-ray diffraction analysis. Fourier Transform Infrared (FTIR) and FT Raman spectral analysis of the crystalline samples reveal that the crystalline sample consist consists of all functional groups. Thermal analysis of the crystalline sample was performed by TGA and DTA methods. The Vicker's micro hardness value was measured for KFCT crystals. The square etch pits with a hopper-like structure is an indicative of 2D nucleation mechanism. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] A solid-state NMR study of phase structure, molecular interactions, and mobility in blends of citric acid and paracetamolJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 5 2009S. Schantz Abstract Citric acid anhydrate (CAA) and paracetamol (PARA), prepared as crystalline physical mixtures and as amorphous blends, were studied using 13C solid-state cross polarization magic angle spinning (CPMAS) NMR. Amorphous blends showed significant line broadening from the conformational distribution as compared to the crystalline samples. Also, chemical shift variations were observed between crystalline and amorphous blends, which were attributed to differences in intermolecular interactions. Averaging of proton rotating-frame spin-lattice relaxation times (T1,) probed via different 13C sites in the amorphous blends confirmed molecular level mixing. For some, initially amorphous, sample compositions the onset of crystallization was evident directly from spectra and from the significantly longer T1, relaxations. Thus, crystallization caused phase separation with properties of the two phases resembling those of pure CAA and PARA, respectively. 13C spectra of amorphous 50/50 (w/w, %) CAA/PARA recorded from above the glass transition temperature broadened as the temperature increased to a maximum at T,,,Tg,+,33 K. This was the result of a dynamic interference between the line narrowing techniques being applied and the time scale of molecular reorientation in the miscible melt. The derived average correlation time was found to correspond well with previous results from melt rheology. We conclude that the underlying reasons for physical instability (i.e., crystallization from the miscible melt, including molecular interactions and dynamics) of this class of amorphous binary mixtures can be effectively evaluated using NMR spectroscopy. © 2008 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 98:1862,1870, 2009 [source] Insights into phase stability of anhydrous/hydrate systems: a Raman-based methodologyJOURNAL OF RAMAN SPECTROSCOPY, Issue 3 2010Mariela M. Nolasco Abstract FT-Raman spectroscopy turns out to be a powerful technique to evaluate the amount of polymorphic and pseudopolymorphic forms in crystalline samples,which is particularly relevant in pharmaceutical sciences. This paper presents a methodology that allows successful quantitative evaluation of the solid-state hydration and dehydration processes, using FT-Raman spectroscopy. All the steps required for a reliable evaluation of the hydration/dehydration process are illustrated for the caffeine system, a particularly challenging system presenting limited spectral differences between the pseudopolymorphs. The hydration process of caffeine was found to occur in a single-step process with a half-life time of ca 13 h, while the dehydration occurs through a two-step mechanism. The critical relative humidity was found to be at ca 81 and 42% for anhydrous and hydrate caffeine forms, respectively. Copyright © 2009 John Wiley & Sons, Ltd. [source] Organic cyclic difluoramino-nitramines: infrared and Raman spectroscopy of 3,3,7,7-tetrakis(difluoramino)octahydro 1,5-dinitro-1,5-diazocine (HNFX)JOURNAL OF RAMAN SPECTROSCOPY, Issue 8 2009Philippe F. Weck Abstract We present the first vibrational structure investigation of 3,3,7,7-tetrakis(difluoramino)octahydro-1,5-dinitro- 1,5-diazocine (HNFX),and, more generally, of a member of the new class of gem -bis(difluoramino)-substituted heterocyclic nitramine energetic materials,using combined theoretical and experimental approaches. Optimized molecular structure and vibrational spectra of the Ci, symmetry conformer constituting the HNFX crystal were computed using density functional theory methods. Fourier transform infrared and Raman spectra of HNFX crystalline samples were also collected at ambient temperature and pressure. The average deviation of calculated structural parameters from X-ray diffraction data is ,1% at the B3LYP/6-311 + + G(d,p) level of theory, suggesting the absence of significant molecular distortion induced by the crystal field. Very good agreement was found between simulated and measured spectra, allowing reliable assignment of the fundamental normal modes of vibration of the HNFX crystal. Detailed analysis of the normal modes of the C,(NF2)2 and N,NO2 moieties was performed due to their critical importance in the initial steps of the molecular homolytic fragmentation process. Copyright © 2009 John Wiley & Sons, Ltd. [source] | |||||||||||||