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991.
Jan Večeřa Žaneta Dohnalová Petr Mikulášek Petra Šulcová 《Journal of Thermal Analysis and Calorimetry》2013,113(1):61-67
Synthesis of rutile pigments is based on solid state reaction and on Hedvall effect, i.e., phase transformation from anatase to rutile. Therefore, it is important to know the thermal behavior of these compounds (the temperature of this change). The goal was to prepare rutile pigments of type Ti1?3xCrxNb2xO2+x/2 by conventional solid state method from titanium dioxide TiO2 (AV-01, anatase), to determine an influence of composition (x = 0, 0.05, 0.10, 0.20, 0.30, 0.50) and calcination temperature (850; 900; 950; 1,000; 1,050; 1,100; 1,150 °C) on color properties of these compounds and to analyze other starting compounds of titanium (hydrated anatase paste TiO2·nH2O, titanyl sulfate dihydrate TiOSO4·2H2O (VKR 611), hydrated sodium titanium oxide paste Na2Ti4O9·nH2O) and their reaction mixtures for x = 0.05 by simultaneous TG–DTA analysis. According to the highest chroma C of color, the optimal conditions for synthesis of these pigments are concentration x = 0.05 and calcination temperature 1,050 °C and higher. It was observed that initial temperature 760–830 °C is needful for a formation of rutile structure. This temperature is the lowest for hydrated Na2Ti4O9 paste (760 °C) and similar for other starting compounds of titanium. 相似文献
992.
Tobias Gruber Wilhelm Seichter Petra Bombicz Ingeborg Csöregh 《Supramolecular chemistry》2013,25(6):537-547
An upper-rim dinitro-substituted calix[4]arene possessing two lower-rim ethyl ester pendant groups (1) has been shown to form solid inclusion compounds with acetone (1:1) (1a), DMF (1:1) (1b), DMSO (1:1) (1c) and n-BuOH (2:1) (1d). X-ray crystal structures of the four complexes 1a–d are reported and comparatively discussed, including isostructurality calculations. Although the solid-state conformation of the dinitrocalix[4]arene moiety, stabilized by two intramolecular O–H…O bonds, is maintained in the four inclusion compounds, and all four co-crystals have similar unit cell dimensions and identical space group symmetries, only three of them (1a–c) are homostructural. Depending on the nature of the guest molecule, either the upper or the lower rim site of the calixarene is involved in the complexation, demonstrating either cavitate- or clathrate-type of supramolecular interactions, respectively. Moreover, due to the different guest recognition modes, the calixarene host in 1d is rotated through a non-crystallographic virtual rotation of 180° within the unit cell, in relation to the host molecules in each of the other three homostructural compounds 1a–c, thus giving rise to supramolecular morphotropism – to our knowledge the first case ever described. 相似文献
993.
Hana Sklenářová Petr Chocholouš Petra Koblová Lukáš Zahálka Dalibor Šatínský Ludmila Matysová Petr Solich 《Analytical and bioanalytical chemistry》2013,405(7):2255-2263
This work describes a comparison of three types of commercial high-performance liquid chromatography silica monolithic columns with different inner diameters and generations of monolithic sorbent: a “classic” monolithic column, the first generation (Onyx? monolithic C18, 100 mm?×?4.6 mm, Phenomenex); a “narrow” monolithic column for fast separation at lower flow rates (Chromolith® Performance RP-18e, 100 mm?×?3 mm, Merck); and a recently introduced “high-resolution” monolithic column, the next generation (Chromolith® HighResolution RP-18e, 100 mm?×?4.6 mm, Merck). Separation efficiency (number of theoretical plates, height equivalent to a theoretical plate and van Deemter curves), working pressure, the symmetry factor and resolution were critical aspects of the comparison in the case of the separation of ascorbic acid, paracetamol and caffeine. The separations were performed under isocratic conditions with a mobile phase consisting of 10:90 (v/v) acetonitrile–phosphoric acid (pH 2.80). Detailed comparison of the newest-generation monolithic column (Chromolith® HighResolution) with the previously introduced monolithic sorbents was performed and proved the advantages of the Chromolith® HighResolution column. Figure
Chromatogram of separation using different flow rates (corresponded to optimal separation conditions); 1 0.5 mL?min-1; 2 0.6 mL?min-1; 3 0.3 mL?min-1 相似文献
994.
Hans-Georg Schmarr Petra Slabizki Charlotte Legrum 《Analytical and bioanalytical chemistry》2013,405(20):6589-6593
Trace level analyses in complex matrices benefit from heart-cut multidimensional gas chromatographic (MDGC) separations and quantification via a stable isotope dilution assay. Minimization of the potential transfer of co-eluting matrix compounds from the first dimension (1D) separation into the second dimension separation requests narrow cut-windows. Knowledge about the nature of the isotope effect in the separation of labeled and unlabeled compounds allows choosing conditions resulting in at best a co-elution situation in the 1D separation. Since the isotope effect strongly depends on the interactions of the analytes with the stationary phase, an appropriate separation column polarity is mandatory for an isotopic co-elution. With 3-alkyl-2-methoxypyrazines and an ionic liquid stationary phase as an example, optimization of the MDGC method is demonstrated and critical aspects of narrow cut-window definition are discussed. Figure
Avoiding chromatographic separation of isotopic standards by fine-tuning the isotope effect allows narrow cut-windows in SIDA based MDGC applications. 相似文献
995.
Julia Cuers Marian Rinken Roland Adden Petra Mischnick 《Analytical and bioanalytical chemistry》2013,405(28):9021-9032
Three hydroxypropyl methylcellulose samples (HPMC1–3, DSMe?=?1.45, 1.29, and 1.36; MSHP?=?0.28, 0.46, and 0.84) were analyzed with respect to their methyl and hydroxypropyl substitution pattern in the polymer chains. Ionization yield of HPMC oligomers in electrospray ionization ion trap mass spectrometry (ESI-IT-MS) is strongly influenced by the hydroxypropyl pattern. Therefore, a sample derivatization procedure, as well as suitable measurement conditions that enable relative quantification were elaborated. Analysis was performed by negative ESI-IT-MS after per(deutero)methylation, partial depolymerization, and reductive amination with m-aminobenzoic acid. Measurement parameters like solvent, trap drive, and voltages of the ion transportation unit were studied with regard to the suitability for quantitative evaluation. Using direct infusion of the samples, strong influence of trap drive and octopole settings was observed. Optimized measurement conditions were used for the determination of the HP pattern of the permethylated samples by direct infusion. The methyl pattern was determined from the perdeuteromethylated samples by high-performance liquid chromatography–electrospray tandem mass spectrometry. For HPMC1, substituents were both found to fit the random distribution model. The other two samples showed pronounced heterogeneity which could be interpreted in more detail by extracting methyl subpatterns depending on the number of HP groups. Figure
Determination of the substituent distribution in hydroxypropyl methylcellulose oligomers by ESI-IT-MS (negative mode) after labeling with m-aminobenzoic acid 相似文献
996.
Dr. Matteo Calvaresi Prof. Mildred Quintana Prof. Petra Rudolf Prof. Francesco Zerbetto Prof. Maurizio Prato 《Chemphyschem》2013,14(15):3447-3453
Carbon Nanotubes, CNTs, have been described as rolled‐up graphene layers. Matching this concept to experiments has been a great experimental challenge for it requires a method to exfoliate graphite, generate ordered and stable dangling carbon bonds, and roll up the layer without affecting the unpaired electrons of the dangling bonds that finally have to zip up in an orderly fashion: A tall order for any synthetic strategy. The combined use of ultrasonication of graphite in dimethylformamide and addition of ferrocene aldehyde just does it! 相似文献
997.
Petra J. van Koningsbruggen Matthias Grunert Peter Weinberger 《Monatshefte für Chemie / Chemical Monthly》2003,134(2):183-198
Summary. The structures of linear chain Fe(II) spin-crossover compounds of α,β- and α,ω-bis (tetrazol-1-yl)alkane type ligands are
described in relation to their magnetic properties. The first threefold interlocked 3-D catenane Fe(II) spin-transition system,
[μ-tris(1,4-bis(tetrazol-1-yl)butane-N1,N1′) iron(II)] bis(perchlorate), will be discussed. An analysis is made among the
structures and the cooperativity of the spin-crossover behaviour of polynuclear Fe(II) spin-transition materials.
Corresponding author. E-mail: koning@iacgu7.chemie.uni-mainz.de
Received April 8, 2002; accepted April 18, 2002 相似文献
998.
Oxanilo-N1-dialkyl-N2-arylamidrazones have been prepared by nucleophilic substitution of the chloride function of appropriate hydrazonoyl chlorides. Relative stabilities of Z- and E-isomers, calculated with the RHF/6-31G∗ ab initio method, range between 0.7 and 2.1 kcal/mol. The Z-isomer is detected to be thermodynamically more stable for studied compounds. X-ray structure determination of 2-dimethylamino-N-phenyl-2-phenylhydrazonoacetamide revealed E- and Z-isomers (ratio 1:1) in the crystal. The different intra- and intermolecular hydrogen bond interactions, which are identified in solid state of compounds, are dissolved in polar solvents. All compounds were found to form E/Z-equilibrium in solution. In some cases E-isomers could be separated and fully characterized. 相似文献
999.
Fausto Barazza Petra Malisan Roberto Carniel 《Communications in Nonlinear Science & Numerical Simulation》2009,14(1):182-193
In this work we investigate the application of the rotation of the coordinate system before applying denoising techniques aimed at improving the H/V spectral ratio for seismic site effects estimation. By this rotation, one can detect the direction of maximum and minimum matching between any couple of orthogonal H/V ratios. The direction of minimum matching should represent the direction of maximum anisotropy of the surface layer or a directional noise. To further improve the method, singular spectrum analysis and WASEE techniques are then applied. 相似文献
1000.