By J. F. Jackson, L. Mandelkern (auth.), Roger S. Porter, Julian F. Johnson (eds.)
Read or Download Analytical Calorimetry: Proceedings of the American Chemical Society Symposium on Analytical Calorimetry, San Francisco, California, April 2–5, 1968 PDF
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Additional info for Analytical Calorimetry: Proceedings of the American Chemical Society Symposium on Analytical Calorimetry, San Francisco, California, April 2–5, 1968
Among the techniques 1"1ost cOmmonly used to date have been volume dilato",etry, microscopy, and infrared spectrometry. All of these techniques have S01"1e limitations when data on percent crystallinity vs. ti1"1e are desired. In dilatometry the large sample required precludes low crystallization te"'peratures due to slow thermal equilibration. Microscopic techniques give only a spherulite growth rate or a relative crystallinity when light extinction techniques are used. Temperature sensitivity of the infra-red absorption bands makes measurement of anything but relative crystallization rates exceedingly co~plicated.
Below 100 Mrads L'I%: for these crystals varies within a few percent of 5b cal/g, but at 300 Mrads it decreases by 14% to 48 cal/g. Figure 3 shows the lowering ofL'l%: which occurs beyond a dose of 100 Mrads for single crystals prepared at 70 0 and 85 0 C. It should be noted that the fraction of unirradiated 85°C crystals which thicken during heating to melt at temperatures above 125 0 C may be estimated from the ratio of the heat absorbed above 125 0 C to the total heat absorbed during fusion.
To anneal the samples, they were heated in the calorimeter at 200°C up to 14 hrs. 5°C/min. Calorimetry Techniques A Perkin-Elmer differential scanning calorimeter, type DSC-l, was considerably modified and improved for these measurements. The major changes, which brought the instrument more in line with the DSC-IB calorimeter, can be listed as follows: 1. 0- ~ DOW STYRON 690 ATACTIC Fig. 1. Comparison of specific heats of Dow atactic polystyrene as received, lower curve, and after a 14 hr. annealing at 200 o C, upper curve.