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  • 1985-1989  (5)
Materialart
Erscheinungszeitraum
Jahr
  • 1
    Digitale Medien
    Digitale Medien
    [S.l.] : American Institute of Physics (AIP)
    Review of Scientific Instruments 57 (1986), S. 39-42 
    ISSN: 1089-7623
    Quelle: AIP Digital Archive
    Thema: Physik , Elektrotechnik, Elektronik, Nachrichtentechnik
    Notizen: A new type of instrument has been designed and built to make Fourier transform nuclear-magnetic-resonance (NMR) spectroscopic measurements at temperatures to at least 1200 °C, with a resolution of about 1 ppm. A sample is rapidly and repeatedly shuttled between the furnace and the radio frequency (rf) coil of the NMR probe (both located within a high field superconducting magnet), spending most of the time in the furnace. During each cycle, a series of rf pulses may be given and a single free-induction decay sampled. The rf coil is located outside of the furnace and is maintained at room temperature despite its close proximity to the sample. Electronic stability and coil "filling factor'' are thus both optimized. The sample temperature drops below that of the furnace when cycling begins, but rapidly approaches a nearly constant value with only small fluctuations. 99% BN has been successfully used as a sample container in experiments on 27Al, 29Si, and 23Na in molten silicates in the system Na2O–Al2O3–SiO2.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Contributions to mineralogy and petrology 90 (1985), S. 101-106 
    ISSN: 1432-0967
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie
    Notizen: Abstract The Fe3+/Σ Fe of twenty-nine experimentally formed, iron-bearing silicate glasses has been determined by wet-chemical and Mössbauer spectroscopic methods from 5–10 mg individual splits of 20–40 mg experimental run products. The wet-chemical and Mössbauer analyses were conducted in two separate laboratories (University of California, Berkeley, and the Geophysical Laboratory, respectively). The Fe3+/Σ Fe ranges from less than 0.2 to 0.96, and the total iron oxide content of the samples, from 2.2 to 34.7 wt %, added as Fe2O3. The interlaboratory comparison shows 70% of the Fe3+/ΣFe analyses from the two methods within the quoted uncertainties (±1 σ) of each other and 83% of the analyses within ±2 σ of each other. Replicate analyses in the current data set result in variations within ±1 σ. These uncertainties are similar to those obtained from several hundred Fe3+/Σ Fe analyses of reequilibrated natural rock and simple system compositions carried out with identical analytical methods in the two laboratories. There is no systematic bias in the results from either of the two techniques. The Fe3+/Σ Fe of silicate glasses can be analyzed, therefore, with equal confidence by either the wet-chemical or the Mössbauer spectroscopic method.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    [s.l.] : Nature Publishing Group
    Nature 314 (1985), S. 250-252 
    ISSN: 1476-4687
    Quelle: Nature Archives 1869 - 2009
    Thema: Biologie , Chemie und Pharmazie , Medizin , Allgemeine Naturwissenschaft , Physik
    Notizen: [Auszug] The apparatus developed for high-temperature liquid-state NMR will be described in detail elsewhere. A sample in a 1-cm diameter boron nitride capsule is rapidly shuttled 15 cm between a furnace and a room-temperature radio frequency NMR coil, spending 10 s in the former and -0.5 s in the latter ...
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Physics and chemistry of minerals 13 (1986), S. 371-381 
    ISSN: 1432-2021
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Geologie und Paläontologie , Physik
    Notizen: Abstract 29Si magic-angle spinning nuclear magnetic resonance (NMR) spectra are presented for seven crystalline phases of the nepheline group: natural nephelines from a plutonic environment (Bancroft, Ontario) and a volcanic deposit (Mt. Somma, Italy), kalsilite, synthetic pure Na nepheline, carnegieite, and two samples of orthorhombic KAlSiO4. In all phases, nearly all of the Si sites have four Al neighbors, indicating nearly complete Al-Si ordering. Excess Si over the 1:1 stoichiometric Si/Al ratio appears to substitute randomly for Al on an ordered lattice, adding Si sites with 3 and 0 Al neighbors in a 3:1 ratio. Various types of structural disorder, including Al-Si disorder, that are reported from some x-ray diffraction studies are probably long range in nature and are due to the presence of ordered domains. In naturally occurring nepheline, the relative abundance of T sites with three-fold local symmetry is maintained at the ideal stoichiometric value of 1/4, even when the K/(K+Na) ratio is substantially lower. This is in agreement with conclusions reached about the average structure from x-ray data. The distinction between the two sites, at least in terms of the local structure that is reflected in 29Si NMR chemical shifts, is lost in a pure Na nepheline sample.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 5
    Digitale Medien
    Digitale Medien
    Springer
    Physics and chemistry of minerals 15 (1988), S. 370-382 
    ISSN: 1432-2021
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Geologie und Paläontologie , Physik
    Notizen: Abstract Silicon-29 magic-angle-spinning NMR spectroscopy has been used to investigate the silicon-aluminum distribution in natural samples of analcite and leucite (before and after heat treatment) as well as a leucite synthesized from a gel. Three different simulation programs have been developed to fit the experimental spectra. For two we assume a different aluminum occupancy fraction g i for each of the three crystallographically distinct tetrahedral sites T i in leucite and some degree of aluminum avoidance, but an otherwise random arrangement of tetrahedral cations. A third program interchanges Al and Si cations on a lattice of 3×3×3 unit cells to generate an optimized fit. All models predict that the T 2 sites in natural leucite are deficient in aluminum: g 1≈0.39, g 2≈0.16, and g 3≈0.42 for the fractional Al occupancy at each site, with apparently strict aluminum avoidance. Heat treatment of the sample at 1673 K for a week has little effect on the g i values but may create some Al-O-Al linkages. In the gel-synthesized leucite, Al occupancies are slightly more uniform than in natural leucite: g 1≈0.36, g 2≈0.20, and g 3≈0.42. For analcite, two distinctly different Si, Al distributions are obtained: (A) g 1=g 3≈0.09, g 2≈0.78 and (B) g 1=g 3≈0.46, g 2≈0.04. Additional NMR measurements on an ion-exchanged sample or an accurate determination of unit-cell dimensions could resolve this ambiguity.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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