OU Crystallography Lab

Department of Chemistry & Biochemistry
Chemical Crystallography Laboratory

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CCD Instrument Alignment Instructions (SMART)

Note that instrument alignment is only to be carried out by the lab director or another trained and designated person. The person performing these tasks should wear eye glasses and the appropriate TLD radiation detectors. When the enclosure must be opened with the shutter open, keep as much of your body as possible shielded from the main beam by the enclosure door. When finished with the alignment, record the work in the log book.

  1. From the SMART program turn down the power to the X-ray generator to 20 kV and 5 mA using the Goniometer/Generator command. Drive all instrument angles to 0° using the Goniometer/Zero command. Exit the SMART program on the PC computer, but leave the computer power on.

  2. Shut down the D8 goniometer by depressing the 0 button on the red rounded column on the right side of the instrument. Note that doing this will also shut down the X-ray generator.

  3. On the X-ray generator control panel, turn on the heater switch. The heater button is the black button between the Off and On buttons on the front of the generator. If the green lamp is not lit, depress and hold the heater button for about 5 seconds.

  4. Turn the switch to the detector power supply to the off position. The detector power supply is located on the top left side of the cabinet behind the lower front panel.

  5. Remove the beam stop and incident-beam collimator. Install the 0.3 mm incident-beam collimator.

  6. Activate the Service key. The service lock is located at the top middle region, behind the lower front panel of the instrument cabinet.

  7. Restart the D8 goniometer system by depressing the 1 button on the rounded right-hand corner of the instrument. The yellow busy lamps on the rounded corners of the instrument base will come on and remain on while the D8 goniometer computer boots. Wait until the yellow busy lamps are off before proceeding.

  8. Turn on electrical power to the detector.

  9. Turn on the X-ray generator by depressing the ON button on the generator. The power should read 20 kV and 5 mA.

  10. On the PC computer start the SMART program. Check the temperature of the detector using the Goniometer/Manual routine and type the letter u. Wait until the temperature of the detector drops down to the range of -41 to -43°.

  11. Open the X-ray shutter using the Goniometer/Shutter routine. Display a ratemeter using the Goniometer/Manual routine and typing the letter c. If the counts are too large, then close the ratemeter with <ESC>, insert the attenuator using Goniometer/Attenuator, and restart the ratemeter. If the counts are too low then exit the ratemeter, close the shutter with Goniometer/Shutter, install the collimator with the next larger size of pinholes, and begin this step again.

  12. Adjust the position of the tube housing and monochromator crystal to maximize the counts on the ratemeter. Adjust the shafts in this order: vertical translation, horizontal translation, twist, and monochromator. Repeat adjustments until the maximum intensity is found. After completing each horizontal adjustment, move the screw slightly in the opposite direction to relieve pressure on the shaft. The vertical adjustment of the tube housing should always be finished on an upward shaft movement. When finished close the ratemeter and the shutter.

  13. If a collimator larger than 0.3 mm was needed, then insert the 0.3 mm collimator, open the shutter, restart the ratemeter, and maximize the intensity of the beam.

  14. Exit the SMART program and log off of the PC computer.

  15. Shut down the D8 goniometer by depressing the 0 button on the right side of the rounded column of the instrument.

  16. On the X-ray generator control panel, turn on the heater switch. The heater button is the black button between the Off and On buttons on the front of the generator. If the green lamp is not lit, depress and hold the heater button for about 5 seconds.

  17. Turn the switch to the detector power supply to the off position.

  18. Turn off and remove the Service key.

  19. Replace the monocap collimator and beam stop. Be sure to center the beam stop on the collimator opening.

  20. Restart the D8 goniometer system by depressing the 1 button on the rounded right-hand corner of the instrument. Wait until the yellow busy lamps are off before proceeding.

  21. Turn on electrical power to the detector.

  22. Turn on the X-ray generator by depressing the ON button on the generator. The power should read 20 kV and 5 mA and the 4 white X-RAY ON lamps will be lit.

  23. Log into the PC computer as the administrator, and start the SMART program. Set the operator Level to 3. Raise the power of the generator to 50 kV and 30 mA. Check the temperature of the detector using the Goniometer/Manual routine and type the letter u. Wait until the temperature of the detector drops down to the range of -41 to -43°.

  24. Collect a quick set of data using the YLID test crystal. From the refined cell and instrument parameters update the x and y beam positions using the Edit/Config command. Also update the ω0 value using the Goniometer/Encoders command. Clear the sample identification and cell parameter information and save these new settings in the smallmol.ini, and protein.ini files using the Crystal/Overwrite Defaults command. Also save the new x and y settings in the c:\saxi\smart32\smartdef.ini file.

  25. Log off of the PC computer as the administrator.

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