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preparation for the diffraction experiment, approximately 10-15 mL of each sample was dehydrated under vacuum (< 10-5 torr). Each sample was heated to the temperature that was used in the prior heat treatment. Samples were heated at a rate of approximately 10 C/min, held at constant temperature for a minimum of 4 hours, then were allowed to cool to room temperature. The samples were transferred to 50 mm long and 15.6 mm wide vanadium cans and subsequently sealed in a helium environment with low water and oxygen levels (< 10 ppm). Neutron diffraction data were collected using the 32 detector BT-1 neutron powder diffractometer at the NIST Center for Neutron Research NBSR reactor (Gaithersburg, MD). Measurements were made using a Ge(311) monochromator with λ = 2.0783(2) Å (1 Å = 10-10 m) at ambient temperature. Data were collected over the range of 1.3 – 166.3° 2θ with a step size of 0.05°. The data collection time for each sample was approximately 8 hours. Rietveld Refinement Neutron powder diffraction data were analyzed using the Rietveld (1967) technique in conjunction with the GSAS (Generalized Structure Analysis System) suite of Larson and Von Dreele (1986). To determine the best expected fit to the data, the LeBail intensity extraction method was first used, in effect simulating a fit with an idealized crystallographic model (Le Bail et al., 1988). Background was fit using a Chebychev polynomial with a variable number of terms (between 8-12). Lattice constants and zero point shifts were then introduced and optimized. The peak asymmetry at low angles was treated using the model of Finger et al. (1994). Scattering factors and lengths were set to standard values for neutral atoms, as supplied in the GSAS package. Initial fractional atomic coordinates for the framework constituents in space group 92PDF Image | PSA USING SUPERIOR ADSORBENTS
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