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Analytical Calorimetry: Proceedings of the American Chemical by J. F. Jackson, L. Mandelkern (auth.), Roger S. Porter,

By J. F. Jackson, L. Mandelkern (auth.), Roger S. Porter, Julian F. Johnson (eds.)

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Extra resources for Analytical Calorimetry: Proceedings of the American Chemical Society Symposium on Analytical Calorimetry, San Francisco, California, April 2–5, 1968

Example text

M. 5%w. /min. The peak temperature was taken as the dissolution temperature, Ts, in accordance with a visual experiment. However, a small number of more nearly perfect crystals might exist beyond the temperature when most disappear. Therefore, a second measure of the dissolution temperature, TSI, was taken as the temperature at which the differential temperature falls to the level of the baseline extended. The results are reported in Table II, with equations for the best straight lines obtained by least squares analysis.

For 40 min. Figure 4 Crystals prepared at 70°C. and annealed at 90°C. for 6 min. 0 toj :0 c::: > >-3 :0 ~toj toj Z >-3 (3 ~ t'"' o r:n r:n <1 i5:: > -sa @ ~ i5:: :0 toj ::t: >-3 ::t: toj H. M. SCHLEINITZ 30 The results for the thermodynamic dissolution temperature agree favorably with those of Coran and Anagnostopoulous (5) and of Peterlin and Meinel (6). They differ from Holland's (7) results, possibly due to solvent or molecular weight differences or possibly because the formation of a thickened border stabilizes the original crystal.

The procedure for r"easurir:g crystalliation rates using the DSC-l is to prepare a fil~ a~out j mils thick of the poly",er to be exa1"1ined. A sa~ple is punched out and crimped into the standard holder, making certain that the bottom of the pan is kept flat. After 1"1aintaining the sample at the desired fusion temperature for the appropriate length of time, the temperature indicator dial is cranked down by hand to the crystallization temperature. Zero ti~e is taken as the ti1"1e when the control light comes on, indicating thermal equilibrium.

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