OCCURRENCE AND DETERMINATION OF LEPIDOCROCITE IN CANADIAN SOILS

1979 ◽  
Vol 59 (2) ◽  
pp. 155-162 ◽  
Author(s):  
G. J. ROSS ◽  
N. M. MILES ◽  
H. KODAMA

Lepidocrocite occurred in B and C horizons of several poorly drained, acid soils; it was determined by X-ray diffraction, electron optical, and chemical dissolution methods. A comparison of X-ray diffraction results obtained by diffractometer, Debye-Scherrer and Guinier-de Wolff methods showed the latter method to be superior in providing the more distinct and complete evidence of lepidocrocite in soil clays. Dithionite-soluble aggregates commonly had a dumbbell-like shape characteristic of lepidocrocite but their electron diffraction patterns were similar to those of maghemite. This suggested the topotactic dehydroxylation of lepidocrocite in the electron microscope. Amounts of lepidocrocite estimated from X-ray diffraction intensities agreed fairly well (within 2.5%) with amounts calculated from iron dissolved by dithionite and oxalate treatments. Lepidocrocite concentrations in soil clays of 1–2% gave distinct X-ray diffraction evidence.

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.


1963 ◽  
Vol 71 (806) ◽  
pp. 63-68 ◽  
Author(s):  
Goro YAMAGUCHI ◽  
Yoshio ONO ◽  
Shigeo KAWAMURA ◽  
Yoshiaki SODA

1993 ◽  
Vol 73 (1) ◽  
pp. 93-102 ◽  
Author(s):  
G. J. Ross ◽  
H. Kodama

The X-ray diffraction (XRD) peak intensities of smectites in Chernozemic and related soils of Western Canada are generally low, in contrast to the high peak intensities of smectites in Podzolic soils of Eastern Canada and those of standard smectite samples. Consequently, X-ray quantitative analysis based on standard smectite samples may underestimate the amount of smectite and overestimate the amount of noncrystalline material in western Canadian soils. This study was undertaken to find the reasons for the weak XRD peak intensities of western soil smectites in terms of their purity and crystallinity. The Tiron dissolution method extracted only small amounts of noncrystalline material from the western soil clays and had little effect on XRD characteristics. The cation exchange capacity (CEC) hysteresis (or pH dependent CEC) between pH 3.5 and 11.0 of the western soil clays was also relatively small which confirmed the absence of significant amounts of noncrystalline material in these soil clays. Observed deviations of XRD positions from true basal spacings indicated that the western soil smectite particles were consistently thinner than the eastern soil smectite and Wyoming montmorillonite particles. Electron microscope observations supported these results. Because the diffraction intensity is proportional to the square of the particle thickness, the thinness of the western soil smectite particles appears to be a major factor in reducing their peak intensities. Thus, to obtain comparable peak intensity data from different soil smectites, particle thickness should be taken into account. Since it is often not practical to measure particle thickness, a procedure for quantifying smectite in soils that avoids this measurement is proposed. Key words: Peak intensity, crystallinity, particle size, particle thickness, Chernozemic smectite, Podzolic smectite


2014 ◽  
Vol 70 (a1) ◽  
pp. C1136-C1136
Author(s):  
Kazuaki Aburaya ◽  
Chiaki Tsuboi ◽  
Fumiko Kimura ◽  
Kenji Matsumoto ◽  
Masataka Maeyama ◽  
...  

A three dimensionally magnetically oriented microcrystal array (3D-MOMA) is attractive to determination of a crystal structure as well as a molecular structure because it does not require a single crystal with sufficient size and quality for diffraction studies. We have developed a novel method to fabricate 3D-MOMA and determined several crystal structures using the 3D-MOMAs[1],[2]. However, the structure determination through MOMA requires a solidification treatment with UV curable monomer prior to X-ray diffraction experiment. We have developed a new X-ray diffractometer equipped with a magnetic field generator, which makes it possible to collect diffraction data without the solidification treatment. In this poster, we describe X-ray diffraction analyses of a magnetically oriented microcrystal suspension (MOMS) of L-alanine without the solidification treatment. A suspension of L-alanine microcrystals was poured in a glass capillary and rotated at a constant speed in a magnetic circuit attached in the X-ray diffractometer. Then, diffraction images were collected every 60 seconds. In the initial phase, the diffraction pattern showed a broad shape similar to that from a powder sample. As time goes on, diffraction patterns have gradually changed to single-crystal like patterns. After 2 hours, the shape of diffraction spots became as sharp as that of a single crystal. This observation shows that the microcrystals are oriented in the same direction. Owing to the improvement of the magnetic circuit and X-ray diffractometer, the quality of the diffraction has been greatly improved compared to that reported previously[3]. Further details of the analyses will be shown in the poster.


2005 ◽  
Vol 61 (1) ◽  
pp. 80-88 ◽  
Author(s):  
Cyril Platteau ◽  
Jacques Lefebvre ◽  
Stephanie Hemon ◽  
Carsten Baehtz ◽  
Florence Danede ◽  
...  

From pure powders of forms I and II of phenobarbital, X-ray diffraction patterns were recorded at room temperature. The starting crystal structural models were found by a Monte-Carlo simulated annealing method. The structures of the two forms were obtained through Rietveld refinements. Soft restraints were applied on bond lengths and bond angles, all H-atom positions were calculated. The cell of form I is monoclinic with the space group P21/n, Z = 12, Z′ = 3. Form II has a triclinic cell, with the space group P\bar 1, Z = 6, Z′ = 3. For both forms, the crystal cohesion is achieved by networks of N—H...O hydrogen bonds along [101]. The broadening of the Bragg peak profiles is interpreted in terms of isotropic strain effects and anisotropic size effects.


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