Rapid scanning with DSC

Experimental details were as follows The sample was contained in a crimped standard Perkin Ehner pan the instrument used was a Perkin Elmer DSC7, with water cooling and nitrogen purging, which had been calibrated to run at the scan rate of 250 K/min. 

The sample had been removed from the filter using dissection tools whilst observing with a light microscope. It had first been placed in a diamond anvil cell for FTIR microspectroscopy, and the infrared (IR)-absorption spectrum, which permitted identification of a polyamide, was obtained. The sample was then recovered from the diamond anvil cell, again with the aid of the microscope and transferred to a pre-weighed sample pan for the DSC experiment. 

These samples were also subjected to some TMA, which reinforced the interpretation of the DSC data and is described below. This experience, as well as demonstrating the value of at least attempting a rapid scan approach with difficult samples, also shows that investigation of derivative curves can be of great assistance in interpreting data, particularly from difficult samples. 

Measurement of the glass transition sometimes causes considerable difficulties if attempted by the conventional heating rate approach to DSC, particularly in the case of formulations carrying heavy loads of filler as either reinforcement or fire retardant. It was desired to determine if a highly filled cable-jacketing material was suitable for low-temperature 

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