PHILIPS X-RAY DIFFRACTOMETER OPERATING PROCEDURE
New Instructions
  1. First, you must be an authorized user trained by JQuinn and EHS
  2. Look for any messages which might prohibit your use. If not, then continue.
  3. Fill out the log-book. Note down initial starting time. This must be where the last person left off. If not, then please email or leave me a note.
  4. Turn Cooling water on.
  5. Load specimen: Do not force the specimen. Only specimens that can fit into the holder should be used. Size specimens appropriately. Close the cover carefully. Again, do not force it since it will damage the shutter switch. If you have a problem, then see me. Also, do not remove any of the sample holders from the room, unless they are YOURS.
  6. Check if kV and mA knobs are at zero position.
  7. Turn generator on.
  8. Turn on computer monitor. The computer should already be on.
  9. On the desktop is software called "PC1710". Start it.
  10. Select a user, such as "first user", "normal user", etc.....
  11. Select "single sample run".
  12. Wait for the software to "intialize" the diffractometer. If it does not, then "abort" and try again.
  13. With ONE MINUTE STEPS, increase voltage in 5kV steps up to 40 kV.
  14. Make sure there is a 1 minute delay after each step.
  15. Increase current slowly to 30 mA. Note: use 30 mA on a regular basis.
  16. Do not exceed 40kV and 30mA.
  17. In the software, set your parameters. This will most likely be 20 degrees to 80 degrees in 0.010 increments, for 1 second/datapoint. The software will calculate the estimated time.
  18. In the software, set the filename. It should be only 8 characters long. Use on A-Z and 0-9. Do not use anyother characters. The file extension should be ".txt". For example "jquinn01.txt" or "nina1234.txt".
  19. Do not set a "comment", this is useless.
  20. After five minutes, you should already be at 40kV and 30mA.
  21. Open Shutter: Press both Shutter and I4 switches together. You press the "shutter button" on the diffractometer the same way you press the "shift", "ctrl", or "alt" key on a computer.
  22. With the shutter open, you can start the scan. The software will change to show you the scanning spectrum. The spectrum will vanish from the screen when finished. However, while it is scanning, you will see the 2-theta angle, d, and intensity.
  23. When finished, you will need to copy the file from the "Xray Data" folder on the desktop to a floppy or zip. The computer does will not use CD or memory key. You could also FTP the file.
  24. Close the software.
  25. Turn off the monitor. Leave the computer on.
  26. Close the #4 shutter.
  27. Slowly turn down the High Voltage and Current over the 5 minutes.
  28. Turn off the generator.
  29. Turn off the water.
  30. Log the final time, subtract the times, and leave a msg if all is OK.
  31. If you have any problems, then please leave a brief message for the other users in the log-book (e.g. "Doesn't Work"). Also, post a sign on the diffractometer and computer. Most importantly, send me an email or hand written messsage with details:
    1. Your name, phone number, room, date, and time,
    2. The problem.
    3. Any actions leading up to the problem.

  32. The use of this equipment is a priviledge, not a right.

  33. Abuse of the equipment or procedures will remove your priviledges.

  34. Tampering, defeating, or adjusting interlocks/limits is STRICTLY forbidden.
    Violaters will be barred from this facility. Additionally, steps will be taken to bar violaters from the department, building, and campus. County and state health-offices will be contacted for the initiation of criminal proceedings.

  35. Remember to:
    1. Wear your x-ray badge (radiation dosimeter)
    2. Turn off the water, when finished.
    3. Properly "log" in/out in the log-book.
    4. Act responsibly.
    5. Return your x-ray badge to the "rack".
  36. Don't mess with the shutter, limits, or electronics

  37. Don't forget to get a copy of PowderCell!
  38. You can also check the PDF (powder diffraction file) on the other computer using various programs, such as Powder-X, X-Plot, X-Powder, etc.....
Old Instructions
  1. First, you must be an authorized user trained by JQuinn and EHS
  2. Look for any messages which might prohibit your use. If not, then continue.
  3. Fill out the log-book. Note down initial starting time. This must be where the last person left off. If not, then please email or leave me a note.
  4. Turn Cooling water on.
  5. Communication with the X-ray computer
    1. We are presently using Kermit to collect our data.
    2. Turn on the computer and monitor.
    3. Once the computer has booted, you will be in the Kermit directory.
    4. Type "kermit" followed by the enter key (<cr>).
    5. Please note: <cr> is the "enter" or "return" key.
    6. Press "cap-locks" to use upper case.
    7. Type "LOG SESSION MYDATA01.DAT" to capture the output of your x-ray spectrum to a file. MYDATA01 should be your name and a series-#, such as jimq231 or aron79. Do not use file names such as iron or copper. Additionally, use the DAT file-extension. Files left on the computer are annually deleted.
    8. Type "C" to connect to the xray computer.
    9. Press <cr> a couple of times.
    10. ***** continue on with the instructions below *****
    11. When your spectrum is complete you must return to the PC.
    12. "^] C"     control right-square-bracket followed by a "C", this will allow you to connect back to the PC, and leave the X-ray computer.
    13. "CLOSE SESSION" will save your data to the hard-drive.
    14. "QUIT" to exit/quit the Kermit program.
    15. "COPY MYDATA01.DAT A:" will copy your data to the floppy drive.
    16. Please remember to check your disk with a Virus-scanner.

  6. Load specimen: Do not force the specimen. Only specimens that can fit into the holder should be used. Size specimens appropriately. Close the cover carefully. Again, do not force it since it will damage the shutter switch. If you have a problem, then see me. Also, do not remove any of the sample holders from the room, unless they are YOURS.
  7. Check if kV and mA knobs are at zero position.
  8. Turn generator on.
  9. The monitor should now read "VS1.5 Terminal="
  10. Hit <cr>
  11. The goniometer will move to 5 degrees
  12. You will get a "C=" prompt on the terminal
  13. With ONE MINUTE STEPS, increase voltage in 5kV steps up to 40 kV.
  14. Make sure there is a 1 minute delay after each step.
  15. Increase current slowly to 30 mA. Note: use 30 mA on a regular basis.
  16. Set parameters. Type "PAR" an the "C=" prompt (Use CAPS LOCK only)
  17. You will see the following screen:

    The following is an example of typical output obtained on entry of the print Parameters command. The information in lower case is explanatory and is not output. 

        LWL 20 UPL 85            setting of detector
                             set lower level at 20%, upper rate at 85%.
    RFS 2E3                  full scale setting of ratemeter 2E3.
    RTC .5 RSP 10 (RTC S)    recorder time constant -5 second,  recorder
                             speed 10 mm/degree.
    SPE 0.02 INT 1.00        scan speed 0.02 deg.,  sampling interval time
                             1 seconds.
    STP 0.050 MXN 10         step size 0.05degrees, number of
                             measurement points on either side of angle.
    MXS 0.010 MXT 2.00       step of 0.01 degrees between measuring 
                             points.  measurement 1 second.
    BGT 5.00 BGM 2           background measurement 5 seconds.  backround 2.
    BGA 0.700 WAV 1.54184    background offset 0.7 degrees. wavelength
                             1.54184.
    SOF ROF DON POF          spinner off.  recorder/ratemeter OFF.  dual
                             output on.  printing recording off.
    ZERO2T -4.990            set the goniometer "ZERO"-position.
    1. Keep LWL and UPL as set
    2. You will NOT be using the recorder
    3. SPE=0.02 , Sets scan speed
    4. INT=1 , Sets sampling time to 1 second per 0.02 deg. Increase counting time if signal is weak.
    5. STP=0.05 , Step size of 0.05 degrees.
    6. MXN=10 Do not change.
    7. MXS=0.01 and MXT=2 Do not change.
    8. BGT=5 Do not change.
    9. BGM=2 Do not change.
    10. BGA=0.7 Do not change.
    11. WAV=1.54184 Do not change.
    12. SOF ROF DON POF, Should read in this manner.
  18. "SAN 20"     [default is 20 deg. start angle. Operator can change this appropriately].
  19. Open Shutter: Press both Shutter and I4 switches together.
  20. "CSC 1"     [scan for 1 degree (20 to 21). check that the scanning time is appropriate, and that you get counts.]
  21. "SAN 20"     [return to your starting angle]
  22. "CSC 60"     [default: This is a continuous scan. Will scan from 20 to 80 degrees. Do not exceed goniometer angle beyond 100 deg. If you need to, please check with the me, and obtain approval.
  23. "\ <cr>"     [abort scan, if necessary (read "slash return")]
  24. "SAN 20"     [to return to the starting angle, when your spectrum is complete.]
  25. "^]C"    [Control right-square-bracket followed by a "C" to return to the PC.]
  26. Continue with the above instructions for Kermit.
  27. Close the #4 shutter.
  28. Slowly turn down the High Voltage and Current over the 5 minutes.
  29. Turn off the generator.
  30. Turn off the water.
  31. Log the final time, subtract the times, and leave a msg if all is OK.
  32. If you have any problems, then please leave a brief message for the other users in the log-book (e.g. "Doesn't Work"). Also, post a sign on the diffractometer and computer. Most importantly, send me an email or hand written messsage with details:
    1. Your name, phone number, room, date, and time,
    2. The problem.
    3. Any actions leading up to the problem.

  33. The use of this equipment is a priviledge, not a right.

  34. Abuse of the equipment or procedures will remove your priviledges.

  35. Tampering, defeating, or adjusting interlocks/limits is STRICTLY forbidden.
    Violaters will be barred from this facility. Additionally, steps will be taken to bar violaters from the department, building, and campus. County and state health-offices will be contacted for the initiation of criminal proceedings.

  36. Remember to:
    1. Wear your x-ray badge (radiation dosimeter)
    2. Turn off the water, when finished.
    3. Properly "log" in/out in the log-book.
    4. Act responsibly.
    5. Return your x-ray badge to the "rack".
  37. Don't mess with the shutter, limits, or electronics

  38. Don't forget to get a copy of PowderCell!
    Old Instructions


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10/25/2004 JQ (originally SS then GL 01/01/98)