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101.
Phosphate (PO(4)(3-)) solutions in water and heavy water have been studied by Raman and infrared spectroscopy over a broad concentration range (0.0091-5.280 mol/L) including a hydrate melt at 23 degrees C. In the low wavenumber range, spectra in R-format have been constructed and the R normalization procedure has been briefly discussed. The vibrational modes of the tetrahedral PO(4)(3-)(aq) (T(d) symmetry) have been assigned and compared to the calculated values derived from the density functional theory (DFT) method for the unhydrated PO(4)(3-)(T(d)) and phosphate-water clusters: PO(4)(3-).H(2)O (C(2v)), PO(4)(3-).2H(2)O (D(2d)), PO(4)(3-).4H(2)O (D(2d)), PO(4)(3-).6H(2)O (T(d)), and PO(4)(3-).12H(2)O (T), a cluster with a complete first hydration sphere of water molecules. A cluster with a second hydration sphere of 12 water molecules and 6 in the first sphere, PO(4)(3-).18H(2)O (T), has also been calculated. Agreement between measured and calculated vibrational modes is best in the case of the PO(4)(3-).12H(2)O cluster and the PO(4)(3-).18H(2)O cluster but far less so in the case of the unhydrated PO(4)(3-) or phosphate-water cluster with a lower number of water molecules than 12. The asymmetric, broad band shape of v(1)(a(1)) PO(4)(3-) in aqueous solutions has been measured as a function of concentration and the asymmetric and broad band shape was explained. However, the same mode in heavy water has only half the full width at half-height compared to the mode in normal water. The PO(4)(3-) is strongly hydrated in aqueous solutions. This has been verified by Raman spectroscopy comparing v(2)(H(2)O), the deformation mode of water, and the stretching modes, the v(1)OH and v(3)OH of water, in K(3)PO(4) solutions as a function of concentration and comparison with the same modes in pure water. A mode at approximately 240 cm(-1) (isotropic R spectrum) has been detected and assigned to the restricted translational mode of the strong hydrogen bonds formed between phosphate and water, P-O...HOH. In very concentrated K(3)PO(4) solutions (C(0) > or = 3.70 mol/L) and in the hydrate melt, formation of contact ion pairs (CIPs) could be detected. The phosphate in the CIPs shows a symmetry lowering of the T(d) symmetry to C(3v). In the less concentrated solutions, PO(4)(3-)(aq) solvent separated ion pairs and doubly solvent separated ion pairs exist, while in very dilute solutions fully hydrated ions are present (C(0) < or = 0.005 mol/L). Quantitative Raman measurements have been carried out to follow the hydrolysis of PO(4)(3-)(aq) over a very broad concentration range. From the hydrolysis data, the pK(3) value for H(3)PO(4) has been determined to be 12.45 at 23 degrees C. 相似文献
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105.
Ahmed El‐Hadi Rainer Schnabel Ekkehard Straube Gert Müller M. Riemschneider 《大分子材料与工程》2002,287(5):363-372
Poly(3‐hydroxybutyrate) (PHB) is sensitive to high processing temperatures. This leads to a decrease in molar mass as well as a lower melt viscosity. The crystallization temperature shifts to lower values, and crystallization kinetics is slow. A mixture was developed in order to improve the manufacturing properties and the final product. The blends exhibit a slight reduction in molar mass because they have a lower melting point than pure PHB, and can be extruded at their melt temperature of 170 to 180°C. Then they immediately crystallize at 125 to 100°C. Differential scanning calorimetry (DSC) shows the effect of holding time in the melt on crystallization behavior. It has been shown that the crystallization time has to be longer in the case of PHB and shorter for the blends. Thermal degradation of PHB and its blends has been investigated using thermogravimetry analysis (TG). Derivative thermogravimetry coupled with TG (TG/DTG) curves show three decomposition stages for blends at 290, 340 and 445°C, respectively. Acetic acid, water, carbon dioxide and methane are produced by degradation at a higher temperature. 相似文献
106.
Here, successful realization of a variable multivariate optical element (VMOE) based on a transmissive liquid crystal (LC) panel is reported. In contrast to conventional multivariate optical elements (MOEs), a single VMOE is a dynamic system, allowing measurement of numerous analytes in different mixtures. Furthermore, VMOE has superior spectral resolution in comparison to a conventional MOE. It is demonstrated here that the system implemented in a Raman spectrometer predicts the concentration of each individual component in toluene-acetonitrile-cyclohexane mixtures with a prediction error of <6% (mass percentage). With a dedicated optical design of the setup, a prediction error smaller than 2% is expected to be feasible for the current chemical system. 相似文献
107.
We have computed the band broadening and the flow resistance in a series of apparently self-similar porous LC support structures, all having the same mean geometric ratios and external porosity, but with a decreasing scale and disturbed by a scale-independent variance on the size and position of the porous solid zone elements. The study shows in a general and qualitative way that each type of LC support that is produced using a manufacturing process displaying a fixed (i.e., domain-size independent) variance on the size and position of the produced solid zone elements will eventually encounter a limit beyond which a further reduction of the domain size can no longer be expected to yield a significant gain in separation speed. This is currently observed in practice for silica monoliths and could also compromise the performance of photolithographically etched columns. 相似文献
108.
Mulder WJ Koole R Brandwijk RJ Storm G Chin PT Strijkers GJ de Mello Donegá C Nicolay K Griffioen AW 《Nano letters》2006,6(1):1-6
MRI detectable and targeted quantum dots were developed. To that aim, quantum dots were coated with paramagnetic and pegylated lipids, which resulted in a relaxivity, r(1), of nearly 2000 mM(-1)s(-1) per quantum dot. The quantum dots were functionalized by covalently linking alphavbeta3-specific RGD peptides, and the specificity was assessed and confirmed on cultured endothelial cells. The bimodal character, the high relaxivity, and the specificity of this nanoparticulate probe make it an excellent contrast agent for molecular imaging purposes. 相似文献
109.
The feasibility of maintenance processes relies on the availability of spare parts. Spare part inventory planning is capital intensive. It is based on demand forecasting, which possesses a high potential in reducing inventories. Even if condition monitoring systems are installed in technical systems, condition monitoring information is barely used to predict the failure probability of units. Therefore, an enhanced forecast model, which integrates SCADA information, has been developed. This leads to more accurate spare part demand forecasts. The approach presented in the paper is based on data mining, the proportional hazards model (PHM) and a binomial distribution. It has been validated with maintenance data of wind energy systems. 相似文献
110.
Ikeda A Hennig C Rossberg A Tsushima S Scheinost AC Bernhard G 《Analytical chemistry》2008,80(4):1102-1110
A multitechnique approach using extended X-ray absorption fine structure (EXAFS) spectroscopy based on iterative transformation factor analysis (ITFA), UV-visible absorption spectroscopy, and density functional theory (DFT) calculations has been performed in order to investigate the speciation of uranium(VI) nitrate species in acetonitrile and to identify the complex structure of individual species in the system. UV-visible spectral titration suggests that there are four different species in the system, that is, pure solvated species, mono-, di-, and trinitrate species. The pure EXAFS spectra of these individual species are extracted by ITFA from the measured spectral mixtures on the basis of the speciation distribution profile calculated from the UV-visible data. Data analysis of the extracted EXAFS spectra, with the help of DFT calculations, reveals the most probable complex structures of the individual species. The pure solvated species corresponds to a uranyl hydrate complex with an equatorial coordination number (CNeq) of 5, [UO2(H2O)5]2+. Nitrate ions tend to coordinate to the uranyl(VI) ion in a bidentate fashion rather than a unidentate one in acetonitrile for all the nitrate species. The mononitrate species forms the complex of [UO2(H2O)3NO3]+ with a CNeq value of 5, while the di- and trinitrate species have a CNeq value of 6, corresponding to [UO2(H2O)2(NO3)2]0 (D2h) and [UO2(NO3)3]- (D3h), respectively. 相似文献