Influence of pH, layer charge location and crystal thickness distribution on U(VI) sorption onto heterogeneous dioctahedral smectite

AbstractThe MudMaster computer program, based on the modified Bertaut-Warren- Averbach (BWA) XRD method, was used in the study of diagenetic evolution of illitic material in shales. The illitic material was characterized by XRD as a mixture of illite-smectite (I-S) and discrete illite. The experimental conditions for complete dehydration of swelling clays, necessary in this method, were established for a climate of high relative humidity (RH >40%). It was found that the distribution of crystallite thickness of dehydrated illitic material of shales is described by the lognormal law, as was established earlier by the BWA method for pure I-S from pyroclastic rocks. The parameters characterizing this distribution evolve with depth: the mean crystallite thickness (Te), the distribution broadening (DW) and the parameter of a lognormal distribution (β2) increase, whereas the percentage of the most frequent crystallite thickness decreases. The observed scatter of values is not random but indicates fluctuations in the characteristics of the illitic material of shales. The results imply that the modified Scherrer technique of measuring mean crystal thickness from the broadening of XRD reflections can be extended at least to some shales.

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Convergent Beam Electron Diffraction

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100070072 ◽

1978 ◽

Vol 36 (3) ◽

pp. 304-315

Author(s):

G. Lehmpfuhl

Keyword(s):

Electron Diffraction ◽

Diffraction Pattern ◽

Crystal Surface ◽

Diffraction Spot ◽

Crystal Thickness ◽

Large Area ◽

Electron Microscopic ◽

Additional Information ◽

Microscopic Investigations

Introduction In electron microscopic investigations of crystalline specimens the direct observation of the electron diffraction pattern gives additional information about the specimen. The quality of this information depends on the quality of the crystals or the crystal area contributing to the diffraction pattern. By selected area diffraction in a conventional electron microscope, specimen areas as small as 1 µ in diameter can be investigated. It is well known that crystal areas of that size which must be thin enough (in the order of 1000 Å) for electron microscopic investigations are normally somewhat distorted by bending, or they are not homogeneous. Furthermore, the crystal surface is not well defined over such a large area. These are facts which cause reduction of information in the diffraction pattern. The intensity of a diffraction spot, for example, depends on the crystal thickness. If the thickness is not uniform over the investigated area, one observes an averaged intensity, so that the intensity distribution in the diffraction pattern cannot be used for an analysis unless additional information is available.

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Computer Indexing of Electron Diffraction Patterns Including the Effects of Lattice Symmetry

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010007775x ◽

1977 ◽

Vol 35 ◽

pp. 22-23

Author(s):

J. S. Lally ◽

R. J. Lee

Keyword(s):

Electron Diffraction ◽

Zone Axis ◽

Crystal Thickness ◽

Double Diffraction ◽

Automated Method ◽

Lattice Symmetry ◽

Intensity Calculations ◽

Unknown Structure ◽

Diffraction Patterns ◽

Orientation Parameters

In the 50 year period since the discovery of electron diffraction from crystals there has been much theoretical effort devoted to the calculation of diffracted intensities as a function of crystal thickness, orientation, and structure. However, in many applications of electron diffraction what is required is a simple identification of an unknown structure when some of the shape and orientation parameters required for intensity calculations are not known. In these circumstances an automated method is needed to solve diffraction patterns obtained near crystal zone axis directions that includes the effects of systematic absences of reflections due to lattice symmetry effects and additional reflections due to double diffraction processes.Two programs have been developed to enable relatively inexperienced microscopists to identify unknown crystals from diffraction patterns. Before indexing any given electron diffraction pattern, a set of possible crystal structures must be selected for comparison against the unknown.

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