PerkinElmer DSC 4000, Инструкция по установке и эксплуатации оборудования

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50 . DSC 4000 Installation and Hardware Guide
Calibrate the DSC 4000
Upon installation, the DSC 4000 must be calibrated for temperature and heat flow before
routine operation. Calibration is accomplished by running high-purity standards or reference
materials with known temperature and energy transitions. The data obtained after running
these materials (that is, temperature transitions and H values) are used in the Pyris
calibration routine to automatically calibrate the analyzer. Once the analyzer is calibrated, it
will remain calibrated, even when the system is switched off, unless there are major changes
to the analyzer’s operating conditions.
The DSC 4000 is shipped with a Spares Kit that contains reference materials. Additional
reference materials can be ordered through www.perkinelmer.com/supplies. Indium and zinc
are generally used for routine calibration.
1. Cut and weigh a small piece of each reference material (indium and zinc), each between
5 and 10 mg. Record the weights.
The DSC 4000 Spares Kit includes precrimped, preweighed samples of indium and zinc
(P/N N5190762). If you use these samples, be sure to use the small sample.
2. Encapsulate the reference material in a standard sample pan.
To achieve the best temperature repeatability, samples should be flattened and placed
in the center of the sample pan, then encapsulated.
3. Using tweezers, place the encapsulated sample into the sample area of the sample
holder (left side); place an empty sample pan and lid into the reference side of the
sample holder (right side).
4. Using tweezers, cover the furnace with the inner and the outer furnace covers.
5. To open the IndCal method from the Method Editor, select
File
,
Open Method
, and
then choose
Indcal.d6m
from the Program Files
\
PerkinElmer\Pyris\Methods directory.
You can also use the calibration method file for zinc called
Zinccal.d6m
.
6. In the Sample Info page, fill in the sample information. Enter the weight of the indium
sample and the file name under which the data will be saved.
7. Click the Start Method button on the DSC 4000 control panel.
The run starts; when completed, the file will be saved with the file name entered in the
method.
8. After the run is complete, perform a Peak Area calculation, include the Onset
temperature and note the Onset result.
9. Repeat steps 1–8 for each reference material you are using to calibrate the DSC 4000.
Up to ten reference materials can be used to calibrate the temperature program of the
analyzer.
10. From the Method Editor, select
Calibrate
from the View menu.
11. Select the Temperature tab.