Stainless steel large volume pans (Perkin Elmer) were fitted with thermally inert silicon rubber rings. These inserts (height
2 mm) were cut from silicon rubber tubing (type S 5/1 SIK 8360) with an internal diameter of 5 mm and a thickness of 1 mm. Starch with 16% water (ca. 25 mg) was then weighed into the pan, which was sealed. Heating scans were performed in a Perkin Elmer DSC 7 or Pyris 1 from 20 C to the selected final temperature at 10 C/min with an empty pan without insert as a reference. After attaining the final temperature the sample was cooled immediately to 20 C at 200 C/min. The pan was opened, the insert was removed by tweezers, and the sample was transferred to a screw-cap tube of known weight by means of a spatula. Maximum final temperature was 210 C. DSC profiles were corrected by subtraction of the profile of an empty pan with insert against an empty pan without insert as a reference. Conventional heating scans were run on samples (50 mg) in pans without insert from 20 to 210 C against an empty pan without insert as a reference.