Step-by-step instructions to use the Bruker D8 advanced research XRD
- If you are the first person to use B2 in the morning allow 15 minutes for mirror to warm up.
- In XRD Commander (Desktop/ XRD Commander) click on Adjust. Use toggle switch to set kV to 40 and mA to 30. Click on Set button. This will bring kV and mA to 40kV and 30mA.
- Open Shutter and wait for 15mins for mirror to warm up.
- Maximum kV and mA settings are: 40 kV and 30 mA.
- Lowest angle you can start from is 1 degree 2-theta.
- Maximum number of counts within 500,000 counts.
- X-Ray window/shutter will not open if doors are not closed properly. Analysis will not start until doors are properly closed.
- Emergency Stop buttons are located on both sides of the instrument. These will shut down the XRD in case of an emergency. Be careful not to touch these while analysis is in progress.
- Do not use solvents and other chemicals that might damage surface of stage.
- Only locked-coupled scans should be carried out. No detector scans!!
Knife edge adjustment
- Close shutter in XRD Commander.
- Open 2 doors of diffractometer.
- Turn on internal light. Green switch below emergency button on left side of instrument.
- Place sample on centre of stage. Use holes as a guide (equal number of holes around sample). Turn on vacuum to hold sample in place.
- Lower knife edge to 0.000mm (knife edge micrometer counter clockwise).
- Raise sample up to knife edge (stage micrometer clockwise direction). Use the torch to watch the gap between knife edge and sample disappear. Make sure knife edge remains at 0.000mm. If number changes it means knife edge is hitting your sample.
- Raise knife edge up to 1.200mm (micrometer clockwise).
- *Close doors. Make sure that ends of both handles fit into holes (clicking sound). If doors are not properly closed X-Ray shutter or window will not open as a matter of precaution. Analysis will not start unless doors are properly closed.
Creation of .dql file for conditions of analysis
- From the Desktop click on XRDWizard.
- Click on File.
- Click on New then choose XRD. Click OK.
- Set 2θ range- Start and Stop angles.
- Set Step size (increment) and Time per Step.
- Scan time is displayed next to generator voltage & current.
- Set kV to 40 and mA to 30.
- File, Save As- browse to your directory in E:\Data\Current Year\Your folder\ to save .DQL file.
Creation of .job file
- In XRD Commander (Desktop/ XRD Commander) click on Jobs.
- Click on the Create Job icon.
- Set the following values:
- Position- 1.
- Sample ID- Description of sample. No restriction as to number of characters.
- Parameter File- Click on 3 dots to browse to E:\ Data\ Current Year\Your folder\ (location of .DQL file created in XRDWizard). Click on file. Open.
- Raw File- Click on 3 dots to browse to E:\ Data\ Current Year\ Your folder\. Create filename for .RAW file. Open.
- Click Start.
- To Save Job File click on Export. Browse to E:\ Data\ Current Year\ Your folder\. Create filename for .JOB file. Save.
- To Open Saved Job File click on Import to browse to E:\ Data\ Current Year\ Your folder\ (location of .JOB file created in Create Jobs). Click on file. Open.
- Open doors.
- Turn off vacuum.
- Remove sample from stage. Clean holder then return to box.
- Close doors properly.
Shut down - end of session
- Close all programs.
- Turn off monitor.