The second phase of calibration involves determination of the cell (enthalpy) constant and the x-axis temperature calibration. This calibration is usually performed using indium and the same ramp rate, purge gas, and pan type as subsequent sample experiments. Cell constant calibration should be performed after a Tzero calibration.
Follow the instructions on the calibration window using the information below as a guideline:
Standard/Weight: Choose the high purity metal standard that will be used for calibration from the drop-down list. The choices include indium (melting point 156.6°C, DH fusion is 28.71 J/g), tin, zinc, lead, mercury, water, and aluminum. Weigh the sample and enter the weight in the appropriate entry field. Recommended size 1 to 5 mg.
Pan
Type/Sample & Reference Pan Mass: Select
the pan type being used from the drop-down list. Aluminum (crimped) pans
are generally used. Other pan choices include aluminum hermetic, gold,
gold hermetic, and "other." "Other" should be used
for all pan types other than those shown. Enter the weights of the empty
sample and reference pans into the appropriate fields (DSC Q2000/Q1000
only). Pan type and weight are particularly significant for Tzero calibration
on a Q2000/Q1000 because they are used to further improve the heat flow
value obtained from subsequent sample experiments by accounting for pan-sensor
heat flow effects. If "other" is chosen as a pan type or if
no pan weights are entered, this correction for pan-sensor heat flow effects
is not applied. See the NOTE below. For more information on DSC pans,
click here Selecting
a Sample Pan.
NOTE: Consideration of pan effects, including the difference in weight between the sample and reference pans, most significantly affects heat flow resolution (i.e., sharper peaks, better segregation of closely occurring thermal events). Because the large weight of the pan and sample when using high volume pans or high pressure capsules decreases resolution, this correction and subsequent generation of T4P heat flow is not recommended.
Post Test: Use this button to access the Post-Test condition parameters that allow you to specify the temperature window once the experiment is complete.
Once all of the experimental parameters are entered, press Next
to proceed to the next step to start the experiment. For information on
the next step click here DSC
Calibration Wizard Constant & Temperature Run.
If you click the Cancel button, the Calibration Wizard is terminated and the cell constant is reset to a value of 1.0.
For information on the Experiment
in Progress window or on results of the calibration experiment
click here DSC
Calibration Wizard Experiment.