TABLE OF CONTENTS A selection of introductory experiments is given below. What can be done will obviously be determined by the apparatus available, and constant reference should be made to the manuals supplied with the instruments. Modern computerized instruments will usually operate interactively, providing some of the directions given in the procedures below. Access to simultaneous techniques and/or evolved gas analysis will add to the possibilities suggested below and provide a great deal more information.
Calibration: Calibrate a DSC with respect to temperature and heat flow. Check on the reproducibility. Compare the results obtained on different instruments, if possible. Carefully compare the calibration procedures given in the respective manuals for power-compensated and heat-flux instruments.
Dehydration: Determine the temperatures and enthalpy changes for the dehydration stages of CuSO 4.5H 2O. Carry out similar measurements on some other hydrates, e.g. BaCl 2.2H 2O, Ni(HCOO) 2.2H2O (formate) or Ni (COO) 2.2H 2O (oxalate) and see how the enthalpy of dehydration per mole of H2O varies from salt to salt. Check the reproducibility of the enthalpy measurements and examine the influence of baseline choice on the values obtained.
Decompositions: Study the decompositions of some metal carboxylates, e.g., Ni (HCOO) 2.2H 2O or Ni (COO) 2.2H 2O, after first having dehydrated them (see 2). Try to carry out an isothermal DSC run at a suitable temperature. Use the data obtained in programmed temperature experiments at different heating rates to estimate...
