Analysis of Highly Exothermic Reactions by DSC

  • A. A. Duswalt

Abstract

In the handling of highly energetic compounds, it is important from a safety standpoint to be knowledgeable about their thermal instabilities. It is sometimes possible to gain information about the sensitivity of a compound by simple inspection of its DTA (or DSC) exothermic decomposition curve. One can, for example, compare the “starting” and maximum peak temperatures of two similar materials, for one of which the stability is known under the conditions in question. This is an admittedly crude test but could be adequate for detecting gross differences, changes during storage, effects of solvent, etc. A more quantitative but still simple test would be to heat a portion of a sample isothermally for a period of time at an appropriate temperature, and then to decompose it, and compare the size of its decomposition exotherm with that of a similar but untreated sample portion. The difference between the two exotherms is a measure of the rate of decomposition of the sample at the isothermal heating temperature. We have used this technique successfully on nitrocellulose formulations as a substitute for the German Test (1).

Keywords

Calorimetry Calorimeter Dition Azide Sulfonyl 

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References

  1. (1).
    Military Standards, Propellants, Solid, Mil-Std. 286 B, July 1966, Method 404.1.2.Google Scholar
  2. (2).
    Frank-Kamenetskii, D. A., “Diffusion and Heat Exchange in Chemical Kinetics”, Princeton Univ. Press, 1955.Google Scholar
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    M. Uricheck, Perkin-Elmer Instrument News, 17, No. 2 (1966).Google Scholar
  4. (4).
    Rogers and Morris, “Analytical Chemistry”, 38, 412 (1966).CrossRefGoogle Scholar
  5. (5).
    Takeo Ozawa, Bull. Chem. Soc. Japan, 38, 1881 (1965).CrossRefGoogle Scholar

Copyright information

© Plenum Press 1968

Authors and Affiliations

  • A. A. Duswalt
    • 1
  1. 1.Research Center Hercules IncorporatedWilmingtonUSA

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