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61.
Eggenhuisen TM den Breejen JP Verdoes D de Jongh PE de Jong KP 《Journal of the American Chemical Society》2010,132(51):18318-18325
We explored melt infiltration of mesoporous silica supports to prepare supported metal catalysts with high loadings and controllable particle sizes. Melting of Co(NO(3))(2)·6H(2)O in the presence of silica supports was studied in situ with differential scanning calorimetry. The melting point depression of the intraporous phase was used to quantify the degree of pore loading after infiltration. Maximum pore-fillings corresponded to 70-80% of filled pore volume, if the intraporous phase was considered to be crystalline Co(NO(3))(2)·6H(2)O. However, diffraction was absent in XRD both from the ordered mesopores at low scattering angles and from crystalline cobalt nitrate phases at high angles. Hence, an amorphous, lower density, intraporous Co(NO(3))(2)·6H(2)O phase was proposed to fill the pores completely. Equilibration at 60 °C in a closed vessel was essential for successful melt infiltration. In an open crucible, dehydration of the precursor prior to infiltration inhibited homogeneous filling of support particles. The dispersion and distribution of Co(3)O(4) after calcination could be controlled using the same toolbox as for preparation via solution impregnation: confinement and the calcination gas atmosphere. Using ordered mesoporous silica supports as well as an industrial silica gel support, catalysts with Co metal loadings in the range of 10-22 wt % were prepared. The Co(3)O(4) crystallite sizes ranged from 4 to 10 nm and scaled with the support pore diameters. By calcination in N(2), pluglike nanoparticles were obtained that formed aggregates over several pore widths, while calcination in 1% NO/N(2) led to the formation of smaller individual nanoparticles. After reduction, the Co/SiO(2) catalysts showed high activity for the Fischer-Tropsch synthesis, illustrating the applicability of melt infiltration for supported catalyst preparation. 相似文献
62.
Campos Giménez E Trisconi MJ Kilinc T Andrieux P 《Journal of AOAC International》2010,93(5):1494-1502
A fast and simple chromatographic method to determine biotin in foods is presented. Biotin is extracted using papain (60 degrees C, 1 h). After pH adjustment and filtration, biotin is determined by LC with fluorescence detection using postcolumn reagent avidin-FITC (avidin labeled with fluorescein isothiocyanate). The method has been validated in a large range of products: milk- and soy-based infant formulas, cereals, cocoa-malt beverages, and clinical nutrition products. The method showed recovery rates of 98.1 +/- 5.7% (average +/- SD) in a large range of concentrations. Biotin concentrations determined in infant formula standard reference materials 1846 and 1849 were in agreement with reference values. RSD of repeatability (RSDr) varied from 2.0 to 4.5%, and intermediate reproducibility (RSD(iR)) from 5.8 to 9.4%. LOD and LOQ were 3.0 and 5.0 microg/100 g, respectively. The proposed method is suitable for routine analysis of biotin in fortified foods (infant formulas, infant cereals, cocoa-malt beverages, and clinical nutrition products). It can be used as a faster, more selective, and precise alternative to the classical microbiological determination, and is easily transferable among laboratories. 相似文献
63.
Renat R. Nazmutdinov Tamara T. Zinkicheva Sergey Yu. Vassiliev Dmitri V. Glukhov Galina A. Tsirlina Michael Probst 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2010,75(4):1244-1252
The structure of sodium cryolite melts was studied using Raman spectroscopy and quantum chemical calculations performed at the density functional theory level. The existence of bridged forms in the melts was argued first from the analysis of experimental Raman spectra. In the quantum chemical modelling emphasis was put on the construction of potential energy surfaces describing the formation/dissociation of certain complex species. Effects of the ionic environment were found to play a crucial role in the energetics of model processes. The structure of the simplest possible polymeric forms involving two Al centres linked through F atoms (“dimers”) was thoroughly investigated. The calculated equilibrium constants and model Raman spectra yield additional evidence in favour of the dimers. This agrees with a self-consistent analysis of a series of Raman spectra for a wide range of the melt composition. 相似文献
64.
Jovica Stojanovi Tamara ?or?evi Ljiljana Karanovi 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(5):i55-i57
The structure of the title compound, ammineaquadi‐μ5‐phosphato‐trizinc(II), [Zn3(PO4)2(H2O)0.8(NH3)1.2], consists of two parts: (i) PO4 and ZnO4 vertex‐sharing tetrahedra arranged in layers parallel to (100) and (ii) ZnO2(N/O)2 tetrahedra located between the layers. Elemental analysis establishes the ammine‐to‐water ratio as 3:2. ZnO2(N/O)2 tetrahedra are located at special position 4e (site symmetry 2) in C2/c. The two O atoms of ZnO2(N/O)2 are bonded to neighbouring P atoms, forming two Zn—O—P linkages and connecting ZnO2(N/O)2 tetrahedra with two adjacent bc plane layers. A noteworthy feature of the structure is the presence of NH3 and H2O at the same crystallographic position and, consequently, qualitative changes in the pattern of hydrogen bonding and weaker N/O—H...O electrostatic interactions, as compared to two closely related structures. 相似文献
65.
Ezhil Jothinathan Kim VanmeenselJef Vleugels Tamara KharlamovaVladislav Sadykov Svetlana PavlovaGeorgia Sourkouni Christian SzepanskiChristos Argirusis Omer Van der Biest 《Solid State Ionics》2011,192(1):419-423
Apatite type rare earth silicates are being extensively studied as electrolyte material for intermediate temperature solid oxide fuel cells (SOFC). In this paper we presents results on synthesis of Al and/or Fe-doped ATLS, the design of compatible anode materials, thermal expansion properties and co-sintering of half-cells from expansion matched materials using the advanced pulsed electric current sintering (PECS) technique. The issues related to the co-sintering of half cells have been addressed successfully by the combined use of nano powders and PECS. 相似文献
66.
We tune optical resonances in rolled-up SiO/SiO(2) microtube cavities by gradually modifying the tube structure through asymmetrical postdeposition of SiO(2). Spectral blueshifts followed by redshifts of the resonant modes are observed in a thin-walled microtube (tube-I), which is attributed to a competition between shape deformation and effective increase of tube wall thickness. In contrast, only a monotonic redshift is detected when asymmetrical deposition is performed on a thick-walled microtube (tube-II). Distinct wavelength-dependent tuning was revealed in both kinds of tubes. Numerical calculations based on perturbation theory are carried out to explain and confirm the experimental results. 相似文献
67.
There is a need for more students to be interested in science, technology, engineering, and mathematics (STEM) careers to advance U.S. competitiveness and economic growth. A consensus exists that improving STEM education is necessary for motivating more students to pursue STEM careers. In this study, a survey to measure student (grades 4–6) attitudes toward STEM and STEM careers was developed and administered to 662 students from two STEM‐focused and three comprehensive (non‐STEM‐focused) schools. Cronbach's alphas for the whole survey and subscales indicated a high internal consistency. Statistically significant difference in means between students attending the STEM‐focused and comprehensive schools on the two subscales of the survey and the overall survey were found. However, the explained variance for these results was approximately 1%. The survey is a useful tool to assess efficacy of STEM education programs on student attitudes toward STEM and STEM careers. 相似文献
68.
S. Selcen Guzey Kristina Tank Hui‐Hui Wang Gillian Roehrig Tamara Moore 《School science and mathematics》2014,114(3):139-149
With the increasing emphasis on integrating engineering into K‐12 classrooms to help meet the needs of our complex and multidisciplinary society, there is an urgent need to investigate teachers' engineering‐focused professional development experiences as they relate to teacher learning, implementation, and student achievement. This study addresses this need by examining the effects of a professional development program focused on engineering integration, and how teachers chose to implement engineering in their classrooms as a result of the professional development. 198 teachers in grades 3–6 from 43 schools in 17 districts participated in a yearlong professional development program designed to help integrate the new state science standards, with a focus on engineering, into their teaching. Posters including lesson plans and student artifacts were used to assess teachers' engineering practices and the implementation in their classrooms. Results indicated that the majority of the teachers who participated in the professional development were able to effectively implement engineering design lessons in their classrooms suggesting that the teachers' success in implementing engineering lessons in their classroom was closely related to the structure of the professional development program. 相似文献
69.
Mutual Diffusion Driven NMR: a new approach for the analysis of mixtures by spatially resolved NMR spectroscopy 下载免费PDF全文
Christian F. Pantoja Jose A. Bolaños Andrés Bernal Julien Wist 《Magnetic resonance in chemistry : MRC》2017,55(6):519-524
We introduce a new approach for resolving the NMR spectra of mixtures that relies on the mutual diffusion of dissolved species when a concentration gradient is established within the NMR tube. This is achieved by cooling down a biphasic mixture of triethylamine and deuterated water below its mixing temperature, where a single phase is expected. Until equilibrium is reached, a gradient of concentration, from ‘pure’ triethylamine to ‘pure’ water, establishes within the tube. The amount of time required to reach this equilibrium is controlled by the mutual diffusion coefficient of both species. Moreover, a gradient of concentration exists for each additional compound dissolved in this system, related to the partition coefficient for that compound in the original biphasic state. Using slice selective experiments, it was possible to measure these concentration gradients and use them to separate signals from all the present species. We show the results acquired for a mixture composed of n‐octanol, methanol, acetonitrile and benzene and compare them with those obtained by pulse field gradient NMR. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
70.
Nataliya F. Lazareva Tamara I. Vakul'skaya Alexander I. Albanov Vadim A. Pestunovich 《应用有机金属化学》2006,20(10):696-705
The introduction of the organosilicon substituent into the α‐position of an amino group results in cardinal change of the amine reactivity irrespective of the coordination state of silicon. Amines R2NCH2SiX3 [R = Me, Et, PhCH2, CH2SiX3; SiX3 = SiMe3, Si(OEt)3, Si(OCH2CH2)3N] easily react with AgNO3, to give the corresponding ammonium salts (R2NH+ CH2SiX3)·NO3?. At the same time, Ag(I) is reduced to Ag(0). The interaction of N‐methyl‐N,N‐bis(silatranylmethyl)amine with AgNO3 has been investigated by EPR spectroscopy. It was proven that the reaction involved a single electron transfer stage with the formation of cation radical of this amine. A mechanism of the reaction is proposed. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献