Design and development of a self-referencing DSC

An intermediate range (50-1000degreesC) self-referencing differential scanning calorimeter (SR-DSC) has been built and its performance evaluated. The SR-DSC measures heat flow across a heat flow metal plate, and any changes to the heat flow caused by a thermal transition occurring in a centrally placed sample is monitored by a temperature difference across the plate. The criteria for high sensitivity are that the circular plate should be as thin as possible and have a low thermal conductivity. The best sensitivity conducive with robust behaviour was achieved with an inconel thermal plate of uniform thickness, 75 mum, this gave reproducible results, and the enthalpy of the thermal transition was proportional to sample mass. Calorimeter sensitivity decreased with increasing temperature and a sloped baseline was observed. Both of these effects can be corrected mathematically. An example of the use of the SR-DSC in polymer characterisation was limited to a study of the physical ageing of PET.