Powder

Follow this procedure if your sample has been crushed to a fine powder. 

1. Sign in to the log-book.

2. Open the Crysalis Pro software. 

3. Select the CMD command shell button (second from top on the left).

4. Type "script" (no quotes) into the command line. 

5. Navigate to C:Xcalibur/macro/

6. Select turn_on_xray_mac.

7. Let the instrument warm up for 1 hour. 

8. After one hour, note the instrument parameters in the log book. 

• •  Write down CCD and X-ray parameters from the right-hand panel.

  •  Minimize the Chrysalis software and open the yellow Tools icon. Select the "details" button for Chiller Flow and X-ray Chiller Flow (actually Chiller Cu). Then          reopen Chrysalis Pro. 

9. Prepare your sample by gluing some of your sample powder to the small polyethylene "Cryoloop."Remove the bottom two segments of the Cryoloop, and place it into the small sample mounts located in the lab. 

10. Place the prepared, mounted sample onto the XRD. 

11. Push F12 on the computer to temporarily move the detector out of the way. Adjust the positioning of your sample using the goniometer wrench, so that it is centered from various angles in the camera. You can use the keypad with the "0" "90" "upper" etc to move the instrument to different angles. When finished, press F12 on the computer. 

12. On the computer, press the CMD icon. Type "sm i 1.0" (no quotes) into the command line and press enter. This is a check to make sure the beam stop is properly aligned. 

13. Push the powder diffraction button and close the command shell. 

14. This opens the powder diffraction window.

• • First navigate to the appropriate folder for the program to store your data. 

  • Change the number of darks to 2 or 3. This is the number of background readings. 

  • Change exposure time to 60-90 seconds to save time. You can leave it longer if you wish. 

  • If you want to further reduce the analysis time, press the "edit runs" button and delete the third line. 

  • Press "Start with Analysis."

15. Analysis will automatically begin, and you will see the red light come on from time to time. 

16. When analysis is finished, the righthand panel will say "CCD ready." It is now safe to open the door, and place your next sample in the XRD.