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- Place a small amount of sample powder in the center of a quartz or single crystal quartz disk.
- Add 2–3 drops of 70 % isopropyl alcohol or distilled water to the sample. Note: Isopropyl dries faster than water.
- Spread the sample to a thin layer using a glass rod. The slurry should be spread evenly across the disk. If there is not enough material to cover the entire disk, concentrate the sample in the middle of the disk where the X-rays will contact the sample.
- Place the sample in the desiccator to dry before running in the XRD.
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Running a regular XRD sample requires the following steps:
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Figure 33. Anti-air scatter screen in place inside the instrument (top image) and after being removed (btm image).
Scanning the NIST 1976 Standard and Verifying QA/QC, homing the axis inside the XRD.
Running the Scan
Run the scan as you would for a sample. With D4 Tools closed, open XRD Commander. Initialize the drives and click on the "Create Jobs" tab. Enter the sample position. The corundum standard does not have a text ID, so name it with an informative convention (e.g., Corundum NIST 1976 X396). Make the sure the name matches the name entered in the "Raw File" column. The parameter file, Corundum QAQC continuous 20 to 130.dql, is found at Local Disk C: >DIFFDAT1. Under the "Raw File" tab, set the path to the DATA>IN folder; this scan will not be uploaded to the LIMS database.
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