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Apparatus for the Oscillating‐Heating Method of X‐Ray Powder Diffraction
Author(s) -
ROWLAND R. A.,
WEISS E. J.,
LEWIS D. R.
Publication year - 1959
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1151-2916.1959.tb14080.x
Subject(s) - dehydration , ethylene glycol , vermiculite , powder diffraction , diffraction , magnesium , sodium , materials science , schematic , analytical chemistry (journal) , chemistry , mineralogy , composite material , metallurgy , optics , chromatography , electrical engineering , crystallography , organic chemistry , biochemistry , physics , engineering
An apparatus for obtaining the X‐ray powder diffraction pattern of a sample while its temperature is increasing at a constant controlled rate has been developed. This equipment is described in enough detail to permit duplicate construction. The program controller is continuously sensitive to the sample temperature and controls the amount of power supplied to the sample heater. Complete schematic details of the electronic circuitry are included, and mechanical details of the program generator are illustrated photographically. The dehydration of clays and related minerals is discussed to illustrate the use of this versatile apparatus. The first order diffraction maxima of water‐wet vermiculite and monoionic sodium, calcium, and magnesium montmorillonites are recorded while the sample temperature is increased at the rate of 5°C. per minute. This is then repeated with ethylene glycol substituting for the water. The temperatures of dehydration and of deglycolation depend on the nature of the exchange cation and are shown to increase in the order sodium < calcium < magnesium.