Degas the Sample

Degas a Single Degas Port

Degassing a single port is useful for degassing samples without using predefined parameter files.

Guidelines for degassing a single port:

  • One degas operation can be started at a time.
  • A sample can be added to any idle port and a degas operation started. When a sample is added, the degas operation in progress will be suspended until the sample reaches the target temperature, then degassing on all ports will resume.
  • Samples can be removed from any of the 12 ports without disturbing the degas operations being performed on other ports.
  • A manual evacuation can be performed on any idle degas port.

  1. Click Browse to select the sample file.
  2. Select the Degas Conditions from the drop-down list.
  3. Select the port to be used for degassing.
  4. Click Start to begin the degas process on the selected port.

Degas on Multiple Degas Ports

Guidelines for degassing on multiple ports:

  • Up to 12 degas operations can be started simultaneously.
  • A sample can be added to any idle port and a degas operation started. When a sample is added, the degas operation in progress will be suspended until the sample reaches the target temperature, then degassing on all ports will resume.
  • Samples can be removed from any of the 12 ports without disturbing the degas operations being performed on other ports.
  • A manual evacuation can be performed on any idle degas port.

  1. For each sample port to be used, click Browse to select the sample file.
  2. Click Start to begin the degas process on the selected ports.

Degas on Analysis Ports

The characterization of microporous materials may be significantly improved by starting the analysis with the sample pre-evacuated. The additional time required is often offset by improved analyses and faster run time. To avoid exposure to contaminants, it is often best to degas a microporous sample on the same port that will be used for analysis.Heating mantles (provided with the micropore option) are required for this type of degassing.

To degas a sample on an analysis port:

  1. With the sample tube mounted in the sample port, position the P0 tube so that it is away from the sample tube.
  2. Slide the isothermal jacket up to the top of the sample tube.
  1. P0 tube
  2. Move isothermal jacket to top of sample tube
  3. Isothermal jacket
  The isothermal jacket fits tightly on the sample tube to ensure thermal stability. Use care when changing the position.
  1. Go to Unit [n] > Evacuate Analysis Port.
  2. Select the port where the sample tube is attached.
  3. Enter the evacuation parameters. Click Start. Repeat the previous steps for each sample to be degassed.
  4. Go to Unit [n] > Enable Manual Control. If the analyzer schematic does not display, go to Unit [n] > Show Analysis Schematic. Ensure a checkmark displays to the left of the Enable Manual Control menu item
  5. When the evacuation for each selected port is finished, ensure valve 8 is left open. See Show Analysis Schematic.
  6. Open the sample ports that are in use. Also open corresponding P0 ports 11 through 16. Open ports 7, 9, and 10. For example, if only four samples are to be degassed and they are on ports 1, 2, 3, and 5, open ports 1, 2, 3, 5, 11, 12, 13, 15, 7, 9, and 10.
  1. Insert the heating mantle thermocouple plug into the thermocouple connector on the degas portion of the analyzer below the sample port. Insert the heating mantle power plug into power connector below the thermocouple connector and twist to lock securely.

  1. Loosen the lace on the heating mantle.
  2. Slide the heating mantle around the sample tube, then tighten the lace.
  3. Secure the heating mantle with a mantle clip.

  1. Go to Unit [n] > Show Degas Schematic.
  2. Right click the degas port where the heating mantle power plug and thermocouple are connected. Select Set. Enter 10 °C/min for Ramp Rate and 200 °C for Target Temperature.

  1. Allow the sample to degas for a minimum of one hour. Additional time may be required to fully degas the sample.
  2. Right click the degas port sample tube. Select Disable.
  Do not touch the sample tube or heating mantle until cooled.Touching the sample tube, heating mantle, or heating mantle clip before they have cooled could result in burns.
  1. When the heating mantle is cool enough to touch, remove it from the sample tube.
  2. Allow the sample to cool to room temperature.
  3. Slide the isothermal jacket down.
  4. Place the sample tube dewar cover over the sample tube stem just above the isothermal jacket. Ensure the P0 tube is next to the sample tube.

  1. Place the safety shield over the sample tube and dewar cover, then begin the analysis. See Perform an Analysis.