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X-ray Diffraction & Scattering
Wide Angle

Siemens D-500

Operation With the Radix Databox and Sample Changer


General
  1. Put your TLD ring on and record the ring number on the computer.
  2. Record your CUFS number, name, time on the hour log (on the goniometer) and the time of day in the computer..
  3. Power up the system:
    • If using colbalt radiation, bring voltage from 10 kV to 38 kV by flipping the switch one kV at a time.  Note: at 19, and 29, flip both the 10's and 1's at the same time.
    • If using copper radiation, bring voltage from 10 kV to 45 kV by flipping the switch one kV at a time.  Note: at 19, 29, and 39, flip both the 10's and 1's at the same time.
    • Bring amperage from 5 mA to 40 mA by flipping the left switch one mA at a time.  Leave the right switch set where it is.
    • The Databox should be on; if not, turn it on.

Sample Preparation
  1. Prepare your sample(s) in the appropriate sample holder(s).
  2. Remove the magazine from the sample changer.
  3. Fill the magazine with your sample holders-notched end towards goniometer.
  4. Close the magazine.
  5. Place the magazine in the sample changer making sure it is pulled up all the way and lock in place.
  6. Check the slits that collimate the x-ray beam.  Roman numerals should be sequential from left to right (I, II & III, II & III, IV, and IV).  Slit widths: 1.0, 1.0, 1.0, 0.15, and 0.15.
  7. Close the door.

Data Collection
  1. Open the Datascan Program.  The program is on the desktop or may be located by activating "Start" (lower left-hand corner), "Programs", "MDI-Apps", and "Datascan".
  2. Check machine calibration: Choose Controller button.
    Does theta read ½ of two-theta?  If not:
    • click on "drive two-theta only" and drive to 20
    • click on "drive theta only" and drive theta to 10
    • click "drive two-theta and theta coupled"
  3. Set up your scan(s):
    1. Choose "Scan" on the toolbar.
    2. Choose the directory your file will be saved in (top bar).
    3. Enter the file name (less than 8 characters, no ".").
    4. Enter the file ID and comments if necessary.
    5. Set up your scan by:
      • Choose the "setup" window.
      • Enter a new scan setting name (or your existing one).
      • Enter the scan settings (for example: 5.0 to 60.0 degrees two-theta, step of 0.04, dwell of 1.0, step scan).
      • Save Setting.
      • Exit.
      • For the sample changer, click on the "sample changer" option at the bottom, and fill in all the filenames and sample ID by clicking "next".
      • Save your setup.
    6. Click on "Go" to begin data collection.  (Clicking on the clock in the upper right corner will tell you how long the runs will take.)
  4. The shutter must be opened manually:
    There are three keys for the shutter control as outlined below:



    Open the shutter by pressing the top, right button.

Data Analysis
    Use "JADE" for data analysis.  Refer to the manual for specific instructions.

When Done
  1. Close the shutter.
  2. Turn off the hour log.
  3. Remove your sample(s).
  4. Leave the Databox on.
  5. If no one is scheduled immediately after you, turn the amperage down to 5 mA by increments of one.  Remember to turn the amperage down first!
  6. Bring the voltage down to 10 kV by increments of 1.
  7. Clean up sample prep area.
  8. Sign out on the computer.


If you accidentally shut down the x-ray generator, see the Startup Instructions and leave a note in the computer comment section.


If you have any questions or are experiencing problems with the instrument, check the Trouble Shooting guide.