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  • 1
    Electronic Resource
    Electronic Resource
    [S.l.] : American Institute of Physics (AIP)
    Review of Scientific Instruments 68 (1997), S. 4521-4524 
    ISSN: 1089-7623
    Source: AIP Digital Archive
    Topics: Physics , Electrical Engineering, Measurement and Control Technology
    Notes: The design of a novel microcalorimetric sample cell which allows rapid transfer of heat from the sample to the cell wall is described. The solid sample is dispersed around the internal walls of the cell. Since the thermopiles of the microcalorimeter are in contact with the outer surface of the cell, the new design of the cell allows rapid recording of the heat generated by the sample. The robust all-metal cell allows in situ sample activation under conditions of high vacuum and at temperatures up to 500 °C. The dispersion of the sample avoids any "deep bed" effects where gas may not be able to diffuse freely to the surface of all of the sample, which may be the case when a thick layer or plug of the sample is used. The cell enables faster acquisition of heat data and minimizes effects of self-heating of the sample. A simple tool, which assists the introduction of the solid sample into the cell and a compact resistor-element, which fits inside the cell for calibration, are described. © 1997 American Institute of Physics.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    The @journal of physical chemistry 〈Washington, DC〉 97 (1993), S. 6465-6469 
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 31 (1993), S. 1064-1071 
    ISSN: 0749-1581
    Keywords: NMR ; 205Tl ; Solid state ; Zeolites A. X and Y ; Thallium ; Frequency-stepped spin-echo integral method (FUSSI) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thallium-205 NMR is reported for several zeolite samples (A, X and Y; hydrated and dehydrated) with thallium(I) exchanged for sodium. Detection at high field (7.05 T) clarifies the spectrum appearance, and it is seen that chemical shift anisotropy (CSA) dominates some of the band shapes. The large CSAs dictate that the spectrum is recorded piecewise by a frequency-stepped spin-echo integral (FUSSI) method. Magic-angle sample spinning has been observed to give only a very minor line-narrowing effect. Threefold-coordinated zeolite A Tl+ sites adjacent to six-membered rings [Tl(1) and Tl(3)] are both assigned to a resonance which has large CSA (δiso 1183, δδ - 1842), while the remaining zeolite A site [Tl(2)] gives an isotropic line shape (δiso 300). Dehydrated zeolite X gives an isotropic peak (δiso 854) which is assigned to the double six-ring Tl(I), and a broader anisotropic resonance which is tentatively attributed to supercage Tl(III). Data for dehydrated zeolite Y indicate that this has a disordered cation distribution.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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