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CSC 6300 N-DSC III
119
Be sure to remove all of the old buffer. In some cases, it will be necessary to clean
the cell before loading the fresh buffer or sample. For example, if you scanned up in
temperature to a point where your buffer decomposed or aggregated, you will need
to remove these by-products by using the cleaning procedure described in Chapter
4, however this is rarely the case. You generally do not conduct any cleaning
procedure between the buffer and sample scans.
Start the Buffer-Sample scans by selecting Run⇒Start from the main menu. The
instrument will scan down at 1°C per minute to 0°C, it will then equilibrate for 10
minutes before beginning to scan up at 1°C per minute (scan 1). When it reaches 85°C it
will again equilibrate at this temperature (10 minutes) then scan down at 1°C per minute
(scan 2). If it is determined that you do not need to clean the instrument after the buffer
scan the sample should be loaded “on the fly” for the best result. That is the method used
in this example.
Loading the Sample on the Fly
As the buffer scans down
in temperature, the pressure
handle should be removed at
about 30°C. At this time the
degassed sample is loaded
into the sample cell while the
calorimeter is still scanning
(Figure 6-5). Use the same
technique to load the sample
cell (right cell) as was used
to load the buffer. The
reference cell does not need
to be reloaded. As you load
the sample in the calorimeter
the µWatt reading will go
off scale. Do not be alarmed;
Figure 6-5: Data offset while loading the sample on the fly.
User’s Manual