Switch the water chiller on by shifting the control box on wall to "on".
Check that water pressure gauge (in wall behind XRD unit) reads >60 psi.
Use small square key to start machine.
Top off liquid N2 dewar. Red light under dewar should be off for operation. Cooling from warm condition takes 2 to 6 hours.
Turn on detector in covered panel on front of machine by flipping power switch up and turning knob completely to right.
Enter 0 for "No" to query about "tube to be warmed up"
Press start button.
Record tube time and date in the red log book.
Wait five minutes before next increase. Start on software issues below.
Check slits. From left to right, standard configuration is 2° and 4° at source and 0.5° and 0.3° at detector.
Wait five minutes before next increase.
A good time for sample prep?
Wait five minutes before next increase.
Lower lid/door of machine; switch off uppermost red button (on vertical face under door).
Click on Scintag-DSMNT icon.
Under "Hardware-manual command-goniometer":
"Do you want to initialize" - Yes
Check goniometer and knobs on machine to confirm correct location -
Click OK if OK. If not, press "Calibrate". Machine should go to next whole degree; put reading in "set axis position" box.
Axes Power to "on" - hum of machine should be audible
Close goniometer window.
Under "File" and "New Event" go to "Scan" and "normal"
Click on "Data Collection", then
On "general",
Use "browse" to set path to folder in which your data will be stored.
Enter name of file
Enter "ID", which allows more information
On "slit", check slits and correct as necessary: 2° , 4° , 0.5° , and 0.3° .
On "Scan", set as desired
Minimum stop size is 0.01°.
Set scan to continuous or step
Enter scan speed as desired - note time scan will require.
Click "set" - blue will change
Save event
Click on "Data Analysis"
Add "print" to list and check file name (if you want a hard copy right away)
Click on "Go from top".
Box at upper right will have button to allow "Real-time display" as scan progresses.
If scan goes offscale, Control-F rescales the profile.
Profile should be printed after scan is complete (if you indicated above).
Under "New Event" go to "Scan" and "normal"
Click on "Data Collection" and "Scan", then
On "general",
Use "browse" to set path to folder in which your data will be stored.
Enter name of file
Enter "ID", which allows more information
On "slit", check slits and correct as necessary: 2° , 4° , 0.5° , and 0.3°.
On "Scan", set as desired
Set range of °2-theta (recalling that CoKα=1.790Å)
Minimum stop size is 0.01°.
Set scan to "continuous" or "step"
Enter speed as desired - note time scan will require.
Click "set" - blue will change
Save event
Click on "Data Analysis" and "Print" (only if you want an immediate hard
copy)
Enter correct file name next to "Browse" or use "Browse"
Use "delete event" to eliminate old events no longer in sequence
If needed, add "print" to list by selecting "-End List-" & clicking "Print"
Click on "Go from top".
Repeat as needed.
Wait five minutes before next decrease.
Turn off detector in plexiglass covered panel on front of machine by turning knob completely to left and flipping power switch off.
Under "Hardware-manual command-goniometer":
Set to 10° 2-theta (5 theta and 5 omega)
Axes Power to "off" - hum of machine should subside
Close goniometer window.
To print any files, use "File . . .Open" in menu and then File . . .Print"
Log off computer by
Closing windows
Go to box at lower left of window -select "Shut Down . . ."
Select "Close all programs, logoff, and leave computer for next user".
Record tube time in the red log book at this point
Hit "stop" and red key-lock button
Switch the water chiller off by shifting the control box on wall to "off".
LBR 24 October 2001 (updated by PAS January 2008)