TGA Dry Run #1 Report

Date Performed: September 7, 2015

Operators: Romnick B. Unabia and Jun Rey S. Lincuna
Description: This is the first dry run of the TGA. The report includes the basic method used to operate
the TGA from the starting up of the equipment until shutting down, the problems encountered and some
comments and initial results.
A. Starting up of the equipments
In starting up, we used the following procedures:
1. Open the Nitrogen tank so that the gauge reading is between 20 kPa 40 kPa.
2. Switch on the compressor.
3. Turn on the chiller using the back switch button. Next, turn it on from the front button. Wait
until the temperature reading is 20.0 C. The stabilization process is about an hour.
4. Turn on the TGA. The green light which is labeled as Power in the TGA lights up. It was
stable and is not blinking which means that the TGA is OK.
5. Turn on the computer.
6. Run the Pyris software. When the software opens, the Start Pyris button appears. Beside
which, there appears another box which indicates the status of the TGA. Double click the
Start Pyris button.
B. Methods used in TGA
We used the following procedures to start the first TGA run:
1. To start, a user should define a Method. The method would include the sample information
and the user defined program that describes the functions/operation that will be performed by
the TGA. Click File New Method. The Method Editor dialog box appears as shown
in Figure 1. Under Sample Info, we filled in the Sample ID which is the name of the
sample, Operator ID which is the name of the operator and the File Name which
indicates the file where the data of the TGA run will be saved.

Figure 1: Method Editor dialog box.

2. We switched to Program, then we set the flow of how the TGA would run. The entire
program can also be seen exactly the same under View Program. The program of our very
first run is shown below. We based this from the one provided by the Perkin Elmer
technician/operator.

Figure 2: The program flow of our first run.

3. Once everything is set, the Method can now be saved: File Save Method.
C. Running the Method/Program
Once the Method is defined, the user can now run the program using the following procedure:
1. Load/place the pan in TGA. In the Control Panel located at the right side of the window,
click the Zero Weight button. See Figure 3, for the important buttons in the Control
Panel.

Start/Stop
Go to Temp

Cooling Air

Sample Weight

Figure 3: The control panel buttons.

Zero Weight

2. Ensure the Sample Temp 50 C and the Status is At Temp. This can be viewed as
shown in Figure 4. If the Sample Temp 50 C then click the Go to Temp button in the
Control Panel.

Figure 4: TGA status panel.

3. Place sample in the pan and then cover. The TGA weighs the sample and the reading is
indicated under Weight in Figure 4. Then, in the Control Panel, click the Sample
Weight button. The value of the Weight that is indicated in Figure 4 should then replace
the value of Weight in the Sample Info section of the Method Editor in Figure 1 and
the Weight % should become 100%.
COMMENT: In Figure 4, once the sample is placed in the pan, the Weight value should
ideally reflect the actual mass of the sample. However, during the actual operation, that
Weight does not give the expected value (only about 5% during the first run) or worse does
not give any value at all (0.000 mg in the second and run) as can be seen in Figure 4. Perhaps,
there could be some problem in the precision balance of the TGA or with the calibration.
4. If the TGA is still reading, wait for the Weight to be equal to the samples weight and the
Weight % to be equal to 100%.
COMMENT: During the actual run, the TGA reading stabilizes only to ~5.66% of the
expected value. This is clearly a big problem that a TGA cannot give an accurate value!
According to Perkin Elmers Technician, the Weight under the Sample Info in the
Method Editor dialog box can be manually inputted. By doing so, the Weight in Figure 4
does not really change (still does not give the accurate reading) but the Weight %. The only
way to change its value and for the Weight% to be equal to 100% is to manually adjust the
value of the Zero under the Sample Info in the Method Editor dialog box. This is what
the Perkin Elmer technician did. As a matter of fact, in the most common concept of
weighing, this is very wrong! The Zero there reflects the weight of the pan (or any other
else in the TGA furnace during calibration) which is set to be the reference value.
5. In the control panel, click the Start button.

6. After a while, a TGA curve will appear on the screen like in Figure 5. The Program Temp
value will change depending on the Program of your Method. The Sample Temp,
Weight and Weight% also change during the run. The TGA curves of the other methods
and runs are in the Appendix.

Figure 5:TGA curve of the first run.

7. The TGA curve can be exported as an ASCII file: File Export As ASCII. Save
the ASCII file to your own folder.
D. Running for the next sample
Before running for the next sample, make sure that the Sample Temp value drops to 50.00 C.
Cooling down may take longer but for a faster cooldown, click the Cooling Air button in the
Control Panel.
E. Shutting down of the equipments
To turn off the TGA, the procedure are followed:
1. Make sure the Program Temp is 50.00 C. Dont turn off at temperature above 50 C.
2. Click Start Pyris button Close All. Wait for all the windows to close.
3. Shutdown the computer.
4. Turn off the TGA.
5. Turn off the chiller starting from the face switch button then to the back switch button.
6. Turn off the compressor.
7. Close the Nitrogen tank.

APPENDIX
TGA DRY RUN METHODS AND RESULTS
A. Method and TGA curve for Dry Run 1

B. Method and TGA result for Dry Run 2