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Table of Contents
1. Preparing the DSC for operation
1.1 Turning on the system
1.2 Checking the DSC configuration
1.2.1 Checking the DSC firmware version
1.2.2 Checking the Pyris software version
1.3 Connecting the peripheral gases
1.3.1 Nitrogen gas
1.3.2 Helium gas
1.4 Filling the cryofill
2. Operating the DSC
2.1 Equilibrating the DSC
2.2 Baseline adjustment
2.3 DSC calibration
2.3.1 Temperature calibration
2.3.2 Heat flow calibration
2.3.3 Furnace calibration
2.3.4 Calibration reference materials
2.4 Running the DSC
2.4.1 Preparing the sample
2.4.2 Inserting the sample into the DSC
2.4.3 Programming your DSC run
2.4.4 Starting and monitoring the DSC run
3. Post processing
3.1 Baseline correction
3.2 Onset calculation
3.3 Peak area calculation
3.4 Specific heat calculation
by
pressing
the
(Step 3) : The Pyris 1 DSC configuration window will appear as shown below. At the time of
installation no gas accessories were included and the only checked box should be for the Cryofill.
Press the Firmware Version button. WARNING : Do NOT press the update Flash EPROM button
unless you are attempting (after having consulted Perkin-Elmer) to rewrite the systems Firmware.
is displayed as the last two digits of an unbelievably long garble of characters. If the version is
incorrect, you must update the firmware after conferring with Perkin-Elmer and receiving adequate
information on performing the procedure correctly and safely.
(Notes) Installation history :
The Pyris 1 DSC was installed in our lab with the factory default firmware version 6.0 and then
upgraded to version 6.4 using a single floppy installation disk.
(Notes) Problems with earlier Firmware versions :
The only problem noticed with older versions is a strange phantom glass transition which occurs at
around -127 degC during measurements. This phantom change occurred even when the sample
pan was empty. This can cause a sudden discontinuity in specific heat measurements before and
after the nonexistent transition.
(Step 3) The Pyris software main window will appear. You should be able to see the Instrument
Viewer and Method Editor windows inside the main window. The Control Panel should also be
embedded on the main window.
(Step 4) From the main window toolbar, select : Help -> About
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GAS FLOW
(Note) Do NOT use nitrogen gas for subambient DSC runs. Nitrogen gas will liquefy at
temperatures near -196 degC or earlier.
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and observe the pressure buildup in the cryofill. Pressure around 9 psi is normal, but should not
exceed 12 psi. If the pressure is too high, reduce the inflow of LN2 accordingly. You will observe
nitrogen gas escaping through the cryofill vent during the filling procedure. If the cryofill was empty
to begin with, the hissing sound can become quite loud. It will recede when the cryofill has been
filled to a certain degree. When the cryofill is almost completely filled, LN2 will sporadically burst
out from the vent. This is a good time to end the filling as described in the next step. Remember to
protect yourself from LN2 freeze burns with cryo gloves and protective garments.
(Step 7) Close the valves in the following order :
LN2 supply tank valve -> Cryofill inlet valve -> Cryofill vent valve
(Step 8) Immediately loosen the cryo line(hose) to prevent pressure build-up inside the line(hose).
One usually maintains the connection on the cryofill inlet valve and loosens only the connection on
the LN2 supply tank valve.
All preliminary setup is now complete and the DSC is ready for operation.
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input box of the control panel and then pressing the manual go to temp button.
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The calibration section describes procedures with which you may yet not be familiar with. Refer to
other portions of this document for the described procedures as required.
All sample measurements for calibration purposes should be repeated at least 3 times and
averaged, using the run procedure you would normally use (cooling rate, temperature range, etc.)
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11. Select the Save and Apply button in the Calibration window to send the new calibration
values to the analyzer and save the current calibration file.
Go on to the next calibration procedure by clicking on its tab or select Close to close the Calibration
window and begin using the new calibration values.
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8. Select the Heat Flow tab. In the Calibration table, enter the name of the reference material
used, the expected H value, the H result just measured, the weight of the reference
material used, and the name of the method file used for the run.
9. Select the Save and Apply button in the Calibration window to send the new calibration
value to the analyzer and save the current calibration file.
Go on to the next calibration procedure by clicking its tab or select Close to close the Calibration
window and begin using the new calibration values.
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Very-high-purity (>99.999%) organic materials can be used to calibrate the temperature when
operating the DSC in the temperature range from 170C. See the table below for a list of
recommended subambient calibration standards that can be used with your DSC. Normally, the two
transition points of cyclohexane and the melting point of water is used for our purposes.
Substance
Transition
Cyclopentane
Crystal
151.16
69.45
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Cyclopentane
Crystal
135.06
4.94
Cyclohexane
Crystal
87.06
79.58
Cyclohexane
Melt
6.54
31.25
n-Heptane
Melt
90.56
140.16
n-Octane
Melt
56.76
182.0
n-Decane
Melt
29.66
202.09
N-Dodecane
Melt
9.65
216.73
n-Octadecane
Melt
28.24
241.42
Hexatriacontane
Crystal
72.14
18.74
Hexatriacontane
Crystal
73.84
60.25
Hexatriacontane
Melt
75.94
175.31
Water
Melt
0.00
333.88
1. The materials listed here, if used for calibration, must be of 99.999% minimum purity as
even small levels of impurity can affect the temperature and/or energy of the transition.
2. If the peaks are not sharp (as in indium), the sample may be impure and the temperatures
you measure may not be correct. Use a higher purity sample or check the purity of the
sample by an alternate technique such as gas chromatography.
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After the DSC has equilibrated (usually more than 2 hours after cryofill has been enabled) you are
ready to perform DSC runs.
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(Step 1) Open the DSC slide cover. The nitrogen shield gas should be flowing.
(Step 2) Remove the platinum sample holder covers using the DSC tweezer. Do not apply too
much force since this may cause the cover holes to deform. Try not to scratch the covers, either.
(Step 3) Insert the sample pan into the LEFT sample holder, and the reference (empty) pan into
the RIGHT sample holder. Cover the holders with their platinum sample covers and close the DSC
slide cover.
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(Step 2) Selecting the Initial State tab, enter the necessary information as shown below.
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Initial temperature : temperature where your run will start. Usually 25 degC
Y Initial : reference value of heat flow. Usually 0.
Purge gas : Set as Helium @ 20 ml/min
Equilibrate temperature : Usually 0.01 degC
Equilibrate heat flow : Usually 0.01 mW
Equilibrate wait time : Usually 15 minutes
(Step 3) Selecting the Program tab, enter the steps your run will consist of. Your run will start with
an initial isothermal condition. Decide how long it will be isothermal in minute durations.
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(Step 4) Press Add a step to include additional steps. Choose either Temperature Scan for
changing the temperature or Isothermal for maintaining a temperature.
(Step 5) If you choose a Temperature Scan step, input the target end temperature and the
cooling/heating rate.
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(Step 6) Select the End Condition button to set how the system should behave after the run is
completed. The DSC temperature usually should return to its load temperature. You can choose to
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turn OFF the Cryofill and Cover heater if you plan to be absent for a long time or if its your last run
for the day and you wont be able to shut off the system when the run is completed. You should
NOT opt to turn OFF the Cryofill if you plan to do another run. Turning OFF the cryofill will make an
equilibration period necessary when you re-enable the cryofill.
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Use the Instrument Viewer window to monitor the DSC. The Y-axis displays the heat flow in
milliWatts and the X-axis can display either the elapsed time or temperature. The X-axis display is
toggled using the T<->t toggle button on the Pyris toolbar.
The graph scale can automatically be adjusted using the Autoscale option under the View menu.
You can also manually change the scale of the Y or X-axis using the axis scale buttons. You can
further zoom into a certain portion of the graph by clicking, dragging, and double clicking on the
desired region.
Wait for the temperature and heat flow to stabilize before initiating your run. It is a good idea to
manually set the temperature to the initial temperature of your run, then wait for stabilization.
Stabilization is normally assumed to have been achieved when heat flow oscillation is within 0.01
milliWatts.
Start your run by pressing the DSC start button. The run will start soon.
3. Post processing
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Open your saved data file. Select the portion of your run you wish to analyze by selecting the step
from the Curves -> Heat Flow menu. Remove the other residual data from the graph by selecting
the unwanted portion and pressing Shift-delete.
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- Right Limit
Enter the right limit for the onset temperature calculation. When the right limit is selected directly
on the curve by clicking on and dragging the rightmost X to the desired position, the value in the
entry field automatically updates.
- Calculate
Closes the dialog box, displays tangents lines on the curve, and displays the Adjust Tangents
dialog box.
- Left Tangent radio button (on Adjust Tangents dialog box)
Activates the left tangent for adjustment. In general, the left tangent corresponds to the point
where the curve begins to deviate from the baseline. Use the Up and Down buttons to adjust the
left tangent line or move the line on the graph.
- Right Tangent radio button (on Adjust Tangents dialog box)
Activates the right tangent for adjustment. For an onset calculation for a typical heating curve, the
right tangent corresponds to the point of maximum slope of the leading edge of the peak. For a
glass transition calculation, the right tangent should be placed at a position on the curve where
there is not much activity since glass transition measures the change in specific heat. For a step
transition calculation, the right tangent should be where the curve starts to go to back to baseline.
Use the Up and Down buttons to adjust the right tangent line or move the line on the graph.
- Calculate (on Adjust Tangents dialog box)
After adjusting the tangents, click on Calculate to close the dialog box, complete the calculation,
and display the results on the curve.
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When you select Peak Area from the Calc menu, the Peak Calculation dialog box appears along
with two Xs. You can use the mouse to drag the X's to the desired location on the peak to set the
limits of the calculation or you can use the keyboard to type in the limits. The limits should
completely encompass the peak transition. Use the dialog box as follows:
- Left Limit
Enter the left limit for the calculation. When the left limit is selected directly on the curve by
clicking on and dragging the leftmost X to the desired position, the value in the entry field
automatically updates.
- Right Limit
Enter the right limit for the calculation. When the right limit is selected directly on the curve by
clicking on and dragging the rightmost X to the desired position, the value in the entry field
automatically updates.
- Baseline
After setting the limits, select the type of baseline to be used in the calculation and displayed :
Standard is a straight, limit to limit baseline.
Sigmoidal baseline can be used when the curve before the transition is at a different level than it
is after the transition. This most commonly occurs in heat flow data. When sigmoidal baseline is
chosen, tangents are drawn from the beginning of each specified limit. You can adjust these
before the calculation is performed. It is recommended that you use the sigmoidal option.
- Other options to include for calculation and display
The Onset value is calculated by finding the intersection of the baseline and the extrapolated
tangent at the inflection point of the leading edge of the peak. The End value is calculated by
finding the intersection of the baseline and the extrapolated tangent at the inflection point of the
trailing edge of the peak. The Peak Height is the distance from the baseline to the peak. You can
select one, two, or all three items. Select Display Limits to have the X,Y values of the left and
right limits also displayed on the curve.
- Area Options
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Select % Area Curve to calculate and display a percent area curve based on the peak area
calculation.
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