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11.
Vasyl' I. Zaremba Dariusz Kaczorowski Galyna P. Nychyporuk Ute Ch. Rodewald Birgit Heying Rainer Pttgen 《无机化学与普通化学杂志》2006,632(6):975-980
New indides Ce3Ge0.66In4.34 and Ce11Ge4.74In5.26 were synthesized from the elements by arc‐melting and subsequent annealing at 870 K. Single crystals were grown through special annealing procedures in sealed tantalum tubes in a high‐frequency furnace. Both compounds were investigated on the basis of X‐ray powder and single crystal data: I4/mcm, La3GeIn4 type, a = 848.8(1), c = 1192.0(2) pm, Z = 4, wR2 = 0.0453, 499 F2 values, 17 variables for Ce3Ge0.66In4.34 and I4/mmm, Sm11Ge4In6 type (ordered version of the Ho11Ge10 type), a = 1199.3(2), c = 1662.0(3) pm, wR2 = 0.0507, 1217 F2 values, 41 variables for Ce11Ge4.74In5.26. The Ce3Ge0.66In4.34 structure shows a mixed Ge/In occupancy on the 4c Wyckoff position. This site is octahedrally coordinated by cerium atoms. These octahedra share all edges, leading to a three‐dimensional network. The latter is penetrated by a two‐dimensional indium substructure which consists of flattened tetrahedra at In–In distances of 291 and 300 pm. The Ce11Ge4.74In5.26 structure contains three crystallographically independent germanium sites. The latter are coordinated by eight or nine cerium neighbors. These CN8 and CN9 polyhedra are condensed to a complex network which is penetrated by a three‐dimensional indium network with In–In distances of 301–314 pm. The 16m site shows a mixed In/Ge occupancy. Chemical bonding in both compounds is dominated by the p elements. Both ternaries studied exhibit localized magnetism due to the presence of Ce3+ ions. The compound Ce3GeIn4 remains paramagnetic down to 1.72 K, whereas Ce11Ge4In6 orders ferromagnetically at TC = 7.5 K. 相似文献
12.
The diffraction peak broadening induced by hydrogen absorption-desorption cycling has been analyzed in four different Laves phase compounds with the C14 and C15 structures. The broadening is due to strain most probably originating from dislocations generated at the interface between the α and β hydride phases in connection with the cell volume difference between the two phases. It has been shown that it is strongly compound dependent. In the case of the C14 structure, the broadening is large and isotropic, and the latter can be related to the isotropy of the elastic constants of the metallic phase. The broadening is less for the compounds with the C15 structure, which can be related to a possibly softer lattice. Better ageing properties after long-term cycling are predicted for this crystal structure. 相似文献
13.
Summary Chiral stationary phases (CSPs) for liquid chromatography were prepared by the way of an activated carbamate intermediate.
The amino group of aminopropylsilyl silica gel was first activated by carbamylation with disuccinimido carbonate (DSC). The
obtained activated carbamate silica gel (ACsil) proved useful as an intermediate for the preparation of urea-type CSPs. The
reaction of ACsil with (S)- of (R)-1-(α-naphthyl)-ethylamine gave naphthylethylurea type CSPs. These CSPs were also obtained
directly from aminopropylsilyl silica gel by its reaction with optically active (S)- or (R)-succinimido 1-(α-naphthyl)ethyl
carbamate (SINEC). Several phenylthiohydantoin amino acid enantiomers and p-bromophenylcarbamyl amino acid enantiomers were
resolved on the CSPs by elution with aqueous mobile phase. 相似文献
14.
By reacting platinum with alkali metals (A = K, Rb, Cs) a new family of binary alkali metal platinides has been synthesized and characterized by chemical analysis, X‐ray powder diffraction, thermal analysis (DTA and DSC), and magnetic measurements. All three compounds exhibit similar XRD‐patterns with strong reflections that can be indexed on the basis of a rhombohedral crystal system (KxPt: a = 2.6462(1), c = 17.123(1); RbxPt: a = 2.6415(1) Å, c = 17.871(1) Å; CsxPt: a = 2.6505(1) Å, c = 18.536(1) Å; x < ½. The a lattice constant is independent on the alkali metal used and of value close to the Pt–Pt distance in NaPt2 (2.645Å). The c parameter increases monotonically with the growing atomic radius of the alkali metal. The average structure of the alloys consists of cubic close packed layers of platinum atoms with layers of disordered alkali metals in between. For all compounds besides the strong reflections small satellites are observed which cannot be indexed together with the rhombohedral peaks in any rational 3‐dimensional lattice. However, these satellites can be indexed as incommensurate modulations within the ab plane (found propagation vectors k = (0.1011, 0.2506, 0) for CsxPt, and k = (0.0168, 0.2785, 0) for RbxPt). 相似文献
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17.
J. S. Bradshaw N. W. Adams R. S. Johnson B. J. Tarbet C. M. Schregenberger M. A. Pulsipher M. B. Andrus K. E. Markides M. L. Lee 《Journal of separation science》1985,8(10):678-683
Contemporary methods for the synthesis of alkyl- and arylsubstituted polysiloxane stationary phases are reviewed. A new, moderately polar phase containing the 3-(4-methoxyphenyl)-propyl group is reported. 相似文献
18.
Summary Polymerisation of bicontinuous microemulsions yields porous monolithic structures with well defined pore sizes that are potentially
suitable for use as stationary phases for capillary electrochromatography (CEC). A variety of pore sizes can be achieved by
altering the composition of the microemulsion, which typically consists of butyl methacrylate (BMA) and ethylene glycol dimethacrylate
(EGDMA) as the polymerisable oil phase. The aqueous phase consists of water, a surfactant (sodium dodecyl sulphate, SDS) and
a co-surfactant (1-propanol). 2-acrylamido-2-methyl-1-propane sulfonic acid (AMPS) is also added to provide charges along
the polymer backbone to allow electroosmotic flow (EOF) to occur. SEM analysis shows that in-situ polymerisation yields a
monolithic structure with a porous topography. Investigations have shown that these monoliths are easy to prepare, robust
and suitable for the separation of phthalates. They generate higher linear velocities than are achieved using the silica based
HPLC packings normally used for CEC. 相似文献
19.
Summary Forming a polymer layer on the surface of siliceous materials is one of the methods for protecting the silica skeleton from dissolution in alkaline mobile phases as well as eliminating the negative influence of silanol groups on separated molecules e.g. proteins. Polysaccharides, especially their derivatives bearing amine groups, can play the role of the surface layer. This paper discusses the possibilities of preparing such a layer by cross-linking a dextran-polyimine mixture (rather than the traditionally used DEAE-dextran) deposited on the surface of the solid material. The results presented prove the utility of synthesized materials as supports for affinity ligands in high performance affinity chromatography or as supports for complexed metal ions in ligand-exchange chromatography. The properties of the sorbents with a polymer layer can be changed both by the composition of the cross-linked mixture and by chemical modification. 相似文献
20.
Carbonate Isostructural Anions [SnX3]5? in the Compounds Rb6[SnX3]O0.5 and Cs6[SnX3]O0.5 with X = As, Sb, and Bi The metallic shining compounds Rb6[SnX3]O0.5 and Cs6[SnX3]O0.5 with X = As, Sb, and Bi were prepared from the melt starting from adequate mixtures of the elements and SnO2. They crystallize in the hexagonal system (space group P63/mmc, No. 194, Z = 2) with the lattice constants mentioned in ?Inhaltsübersicht”?. In the structures of the isotypic compounds tin and the main group(V) elements build up trigonal planar anions [SnX3]5? with X = As, Sb, and Bi isostructural to the carbonate anion, oxygen forms isolated O2? ions. The bond lengths Sn? X are significantly shortened with respect to the sums of Pauling covalent radii. The atoms of the units [SnX3]5? are coordinated by alkali metal cations forming trigonal prisms and the O2? anions occupy octahedral holes. 相似文献