MAT E 214

Structural Characterization of Materials

Thermogravimetric Analyzer

Perkin Elmer TGA 7 Operating Procedures

Room temperature to 950C

  1. Open the logbook and write down the date, your name, which instrument used (1 or 2), what materialis being run, the sample purge gas, and the temperature schedule (range & heating rate). Also indicate how many runs are performed and any problems that occur.
  1. Open the valve on the Nitrogen cylinder and make sure the output pressure is at 50 psi, also open the valve on the Air cylinder and ensure the pressure is at 40 psi.
  1. Log onto the computer using your CLUE account. The upper left-hand of the screen will have icons for both TGAs – click on the one that corresponds to the machine you intend to use to start the instrument control software.
  1. Select the window that is titled Method Editor. Enter in the name of the sample, the operator’s name, and any comments about the sample. Place the cursor in the File Name box and click on browse. Move to the folder in which you would like the data to be saved and choose a descriptive a file name (e.g. material, atm, operator, and date indicated in file name). Click on save.
  1. Click on the Program button in the method editor window. Click on the add a step button and add a temperature scan. Highlight the Hold for 1.0 minute and click on delete this step button and delete it. At the bottom of the box, enter the final temperature for the scan (max of 950C), and the heating rate desired for the experiment.
  1. Click on the Initial State Button – make sure that baseline subtraction is not selected.
  1. Go to the TGA. Put the empty sample pan in the hanger and slowly move the black platform up to the same height as the hook. Then swing the platform underneath the hook and slide the pan and hanger over the hook. Swing the platform all the way out of the way.
  1. In the software push the raise furnace button. Go to the gas control station and enter the following sequence: run – manual – N2 – start. Just push the button below each option.
  1. Back in the software, check that the weight has stabilized and press the get zero weight button. This will zero the balance. Lower the furnace, and carefully slide the pan and hanger off the hook.
  1. Place the sample in the pan and return the sample and hanger to the hook. Raise the furnace. Also, swing the heat shield down into place.
  1. Wait for the weight to stabilize again and press the get sample weight button.
  1. Enter the starting temperature and push the go to temp button.
  1. Wait for the temperature to stabilize and press the experiment start button.
  1. When the experiment is done, the furnace will automatically lower, remove the sample and hanger from the hook and place on top of the TGA.
  1. If you are the last to be using the TGA, turn off all gases and close the software.

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