Methods of Preparation and Control of Clay Mineral Specimens in X-Ray Diffraction Analysis

I. H. Milne and C. M. Warshaw1
Gulf Research and Development Company, Pittsburgh, Pennsylvania
1 Publication authorized by Executive Vice-President, Gulf Research and Development Company.

Abstract: The determination of the clay minerals present in mixtures by x-ray diffraction examination of oriented aggregates on glass slides becomes more reproducible and more conclusive when the relative humidity of the air in contact with the specimen is controlled during the recording of the diffraction pattern. The basal diffraction peaks of expanding and partially expanding clay minerals vary considerably in spacing and intensity with normal variations of relative humidity. These variations may be eliminated by the application of a simple modification to standard x-ray equipment. This modification is useful in maintaining a constant relative humidity at values between <1 and 100 percent. Dry air is used to maintain the effects of dehydration by heat and, in many cases, may be used as a substitute for heat treatment. This is especially true for mixed-layer minerals, which give more intense and more reproducible diffraction effects in dry air. Wet air is better, in many instances, than glycerol or ethylene glycol in resolving the basal reflections of montmorillonite and illite in mixtures. More information can be obtained from preparations of mixed-layer minerals and mixtures of clay minerals by recording the diffraction pattern at various stages of hydration.

Clays and Clay Minerals; 1955 v. 4; no. 1; p. 22-30; DOI: 10.1346/CCMN.1955.0040104
© 1955, The Clay Minerals Society
Clay Minerals Society (www.clays.org)