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61.
Four new stationary phases for HPLC were prepared by modifying silica gel with a trifrnctional aminoalkyl silane. A conjugated π-electron system was linked to the amino group either directly or with a carboxylic anhydride as a spacer in between. Characterization and dynamic measurements of the new stationary phases were performed by solid state NMR spectroscopy. The results of the 29si and 13C CP/MAS techniques were compared with the recently developed 1H MAS-only technique. Despite strong homonuclear dipole-dipole interactions it was possible to obtain well resolved 1H MAS spectra of those stationaru phases with a high degree of crosslinking. Limited mobility of the aromatic ligand fragments is common for all examined stationaryu phases. The chromatographic properties of the new phases were tested by their ability tio sepatate a mixture of eight PAHS. It could be shown that the π-π interaction mechanism is responsible for the separation of the eight PAHs, because the elution order of the PAHs did not changem despite the use of both a nonpolar mobile phase (n-heptane) and a polar mobile phase (methanol/ water mixture). 相似文献
62.
In this paper the equation for thin-layer adsorption chromatography with multicomponent mobile phases, proposed by O?cik in 1965 is extended to energetically heterogeneous solid surfaces. Other forms of this equation, more convenient in practical applications, are presented. Model calculations are made for TLC with binary mobile phases according to the modified form of O?cik's equation. Finally, this equation is compared with that of Snyder. 相似文献
63.
M. Baru A. Danilov I. Vagenina E. Gorbunova S. Moshnikov L. Mustaeva V. Cherskii 《Chromatographia》1997,45(1):351-354
Summary The design of new dynamic, axial-compression columns with a system for continous packed bed adjustment and monitoring of the
floating adapter position is described. The columns are meant for liquid chromatography at low pressures (up to 8 bar) in
aqueous and organic media with stationary phases of all types. The columns have adapter position pickups for continuous automatic
monitoring of the bed height (original “swellographic” monitoring). The column described with gas pressurisation was tested
with soft Sephadex G-10 and G-25. In spite of the reduction in external porosity there was no dramatic increase in back-pressure.
The column proved to provide long-term stability of the packed bed and improvement in resolution.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
64.
Quanwei?Yu Jens?Fr?mmel Thomas?WolffEmail author Karel?Procházka 《Colloid and polymer science》2004,282(9):1039-1043
Solid stoichiometric complexes of [3,12]-ionene and dodecyl sulfate form upon reaction of the bromide of the ionene and the silver salt of dodecyl sulfate in methanol. IR, DSC, and TG investigations indicated that the solid complexes are stable between 30 and 120 °C. TG and DSC also showed that the complexes easily take up water at ambient conditions. These samples are optically isotropic. When exposed to an increased humidity they exhibit optical anisotropy, i.e., birefringence, which is caused by the formation of a hexagonal mesogenic phase. Mesogenicity is necessarily accompanied by a further uptake of water (4–5 H2O molecules per ionic unit), which is dependent on the relative humidity. The phase behavior as a function of temperature and controlled relative humidity was studied using birefringence measurements and polarizing microscopy. 相似文献
65.
A. Meddour J. Courtieu W. Abdelhadi S. Guermouche M. H. Guermouche 《Chromatographia》1996,43(7-8):387-392
Summary Comparative gas chromatographic properties of two thermotropic Poly(L-glutamates) with long alkyl side chains (10 and 16 carbons called Poly 10 and Poly 16 respectively) are studied.Their thermal properties were established with differential scanning calorimetry (DSC) and gas chromatography. They present a cholesteric liquid crystal in a large temperature range.The chromatographic separation abilities of the two polymers in the liquid crystal state were studied using capillary glass columns. Interesting analytical performances were obtained in different fields: isomeric separation of alkanes, aromatics, polyaromatics, volatile aroma compounds and cis and trans isomers. Some differences were noticed in their behaviours; 2 and 3-methyloctane and xylene isomers are separated only on Poly 10 while limonene and eucalyptol are separated only on Poly 16. 相似文献
66.
Sameena Ashraf Keith D. Bartle Anthony A. Clifford Robert Moulder 《Journal of separation science》1992,15(8):535-538
Lubricating oil additives have been analyzed by supercritical fluid chromatography on open tubular and packed capillary columns. Carbon dioxide and modified carbon dioxide were used as mobile phases and detection was accomplished by flame ionization and micro UV. Rapid and efficient analysis of the lubricating oil additives was demonstrated. 相似文献
67.
L. -M. Yuan R. -N. Fu S. -H. Gui X. -T. Xie R. -J. Dai X. -X. Chen Q. -H. Xu 《Chromatographia》1997,46(5-6):291-294
Summary The gas chromatographic separation of xylene isomers using special mixed stationary phases consisting of heptakis(2.3.6-tri-O-pentyl)-β-CD-AgNO3, heptakis (2.3.6-tri-O-pentyl)-β-CD-TINO3 or bentone-34-AgNO3 is investigated. The first two have positive synergistic effects for the separation of m, and p-xylene isomers, but negative
synergistic effects for the m, and oisomers. The separation effects depend on temperature, mixing ratio and how mixing is
accomplished. 相似文献
68.
O. N. Litvinenko A. N. Kuznetsov A. V. Olenev B. A. Popovkin 《Russian Chemical Bulletin》2007,56(10):1945-1947
Three new mixed tellurides of nickel and group 13–14 metals Ni3−δMTe2 (M = Sn, In, Ga) were prepared by high-temperature ampoule synthesis and studied by powder X-ray diffraction analysis. The
compound Ni3−δSnTe2 was also studied by single crystal X-ray diffraction analysis. The structural model of this phase and two analogs was described
as consisting of layers with nickel-main group metal bonds confined from the above by tellurium atoms. The van der Waals gap
formed through contacts between the tellurium atoms of neighboring layers is partially occupied by nickel atoms.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1879–1881, October, 2007. 相似文献
69.
T.?GrygarEmail author T.?Rojka P.?Bezdi?ka E.?Ve?erníková F.?Kovanda 《Journal of Solid State Electrochemistry》2004,8(4):252-259
Mixed Cu,Mn, Cu,Mn,Al, Cu,Mg,Mn, and Cu,Mg,Mn,Al oxides were obtained by calcination of amorphous basic carbonate (Cu,Mn oxides) or hydrotalcite-like precursors at 300–800 °C. The product composition was characterized by chemical analysis, XRD, and voltammetry of the microparticles. The XRD amorphous portion was detected indirectly by XRD and directly by voltammetry. Tenorite (CuO) and spinels were the main crystalline components of the oxide mixtures. The presence of Al shifted the onset of the crystallization of XRD-detectable tenorite and spinel to temperatures higher by 100–200 °C, and the presence of Mg shifted tenorite crystallization by 100 °C, but voltammetry was able to detect these phases even in XRD-amorphous or nanocrystalline calcines. Voltammetry is hence suitable for analysis of poorly crystalline oxides that can be used in heterogeneous catalysis. 相似文献
70.
R. V. Golovnya 《Chromatographia》1979,12(8):533-538
Summary Equations modifying Rohrschneider's relationship between I and thermodynamical characteristics values are derived. Polarity in chromatography is discussed as a possibility of stationary phases or absorbents to enter into intermolecular interactions and is determined on the basis of the partial molar free energies of solution (G) of six test substances. A simple method for the calculation of stationary phase polarity in terms of G from retention indices and McReynolds constants is given. Equations are presented for the calculation of stationary phase selectivity utilizing G data tabulated for selected test substances. The thermodynamical basis of selecting a reference phase for a unified system expressing the selectivity of stationary phases which can also be applied for adsorbents is suggested. The energy equivalent to an index unit, Gi.u., is discussed. 相似文献