By J. F. Jackson, L. Mandelkern (auth.), Roger S. Porter, Julian F. Johnson (eds.)
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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
It was found that an irradiation dose of 26 Mrads suppressed lamellar thickening of crystals grown isothermally at 85°e in xylene so effectively that nearly 90% of the crystals melted sharply within a 30e temperature interval. We decided to utilize this technique of linking lamellae together in an attempt to measure accurately the melting temperatures of solution grown crystals of various thicknesses. From the information obtained in these experiments we intend to estimate an equilibrium melting temperature, independent of crystal size effects, and to calculate the chain folded surface free energy of the crystal.
A switch for changing the temperature ranges and trimpot controls to adjust the temperature range and span were added to the rear panel of the control cabinet. 6. A Texas Instrument Servo-riter recorder was used and along with it a series of plug-in cards was constructed to enable a quick and accurate change of the recorder scale to be made. 0 and 10 mv. The following experimental techniques and precautions were followed: 5. 1. 2. 3. 4. 5. 6. 7. 8. 9. The recorder, control cabinet and analyzer section were mounted on sponge rubber, Berry shock mounts and Styrofoam, respectively, to reduce vibrations.
Temperature sensitivity of the infra-red absorption bands makes measurement of anything but relative crystallization rates exceedingly co~plicated. With calorimetric techniques, however, percent crystallinities may be calculated as a function of time at a wide range of te'"1peratures provided the heat of fusion of the polymer is known. Sample sizes for the DSC-l are s1"1all, (about 5 mg is sufficient) allowing rapid ther",al equilibration, and the sample temperature can be changed rapidly. The combination of these two capabilities allows crystallization rates to be measured at lower temperatures than on a dilatometer, where sample sizes are on the order of 1 g.
Analytical Calorimetry: Proceedings of the American Chemical Society Symposium on Analytical Calorimetry, San Francisco, California, April 2–5, 1968 by J. F. Jackson, L. Mandelkern (auth.), Roger S. Porter, Julian F. Johnson (eds.)