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The Rapid Simultaneous Measurement of Thermal and Structural Data by a Novel DSC/XRD Instrument

Published online by Cambridge University Press:  06 March 2019

T. G. Fawcett ,
C. E. Crowder ,
L. F. Whiting ,
J. C. Tou ,
W. F. Scott ,
R. A. Newman ,
W. C. Harris ,
F. J. Knoll  and
V. J. Caldecourt
T. G. Fawcett
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
C. E. Crowder
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
L. F. Whiting
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
J. C. Tou
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
W. F. Scott
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
R. A. Newman
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
W. C. Harris
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
F. J. Knoll
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
V. J. Caldecourt
Affiliation:
Michigan Applied Science and Technology Laboratories The Dow Chemical Company Midland, Michigan
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Extract

Over the past 25 years, numerous studies utilizing both X-ray diffraction (XRE) and differential scanning calorimetry (DSC) have been reported In the literature. Generally, conventional high-temperature X-ray data identifies solid-state transitions, then attempts to correlate them with thermal events observed by the calorimeter. Since changes occur in the sample during studies such as these, separate portions of the sample must be used for XRD and DSC experiments. When comparing results of the two experiments, questions arise concerning sample homogeniety as well as temperature and environmental differences. In fact, no conventional high-temperature X-ray diffraction instrument can give the precise control over temperature and heating rate available with a DSC, The problems of sample inhomogeneltles and Instrumental differences could be avoided if X-ray diffraction and DSC could be performed simultaneously on one sample.

Type
VII. New Techniques and Instrumentation in XRD
Information
Advances in X-Ray Analysis , Volume 28: Thirty-Third Annual Conference on Applications of X-ray Analysis, July 30 - August 3, 1984 , 1984 , pp. 227 - 232
Copyright
Copyright © International Centre for Diffraction Data 1984

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References

1.The instrument and method described in this report are the subject of a United States Patent Application.Google Scholar
2. Newman, R. A., p. Moore Kirchhoff, and Fawcett, T.G., “Evaluation of Straight and Curved Braun Position -Sensitive Proportional Counters on a Huber-Guinier X-ray Diffraction System”, Adv. in X-ray Analysis. 27:261 (1983).Google Scholar
3. Fawcett, T. G., Moore Kirchhoff, P., and Newman, R.A., “The Measurement of Thermally Induced Structural Changes by High Temperature (900°C) Guinier X-ray Powder Diffraction Techniques”, Adv. in X-ray Analysis, 26:171 (1982).Google Scholar