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Training and maintenance videos can be found on the XRD technician computer, Desktop/XRD_ICP Prep Documents/Bruker TRAINING VIDEOS

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1. Flip the "On" switch (Figure 1C) to the HASKRIS and the water in the tank will begin to cool. The water temperature needs to reach 69°F (Figure 1A). The Haskris temperature can range between 65°F to 69°F. Ensure all water valves to/from haskris are open.
   
   

   

   Figure 1. HASKRIS Control Panel. (A) Actual temperature. (B) Set temperature. (C) On/Off switch. (D) Flow meter

   
   
   
2. Flip the ON switch (Figure 2A) on the side of the machine.
   1. The solid green "Low Voltage Ready" light (Figure 2F) turns on.
   2. You will hear several beeps and the "System Activity" light (Figure 2D) will start flashing green.
3. Press the "High Voltage Enable" button (Figure 2B).
   1. The "System Activity" light turns green.
   2. An orange "High Voltage Ready" (Figure 2E) light will turn on.

Figure 2. Side control panel on D4 XRD. (A) Power On/Off. (B) High voltage enable button. (C) Alarm light. (D) System activity flashing light. (E) High voltage ready light. (F) Low voltage ready light.

4.      Go to the front of the machine and press the green circular button. This enables the mains power and activates the sample handler (see Figure 4). 

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1. Unless the sample material is very small, select the appropriate sample holder (see Sample Slurry/Smear Slide Mounting for Small Sample Amounts).
2. Label the sample holder with a unique identifier to keep the samples organized (e.g., text ID or 14H2 77-78)
3. Place enough powder from the labeled sample bottle to fill an empty sample holder. Gently press the powder flush with the sample holder using a glass slide. Roll the glass slide over the powder to fill any gaps in material and smooth the surface of the powder. The surface of the powder must be smooth. Remove excess powder from the sample holder edges and carefully place the holder in the D4 sample magazine.

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1. Place a small amount of sample powder in the center of a quartz or single crystal quartz disk.
2. Add 2–3 drops of 70 % isopropyl alcohol or distilled water to the sample. Note: Isopropyl dries faster than water.
3. 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.
4. Place the sample in the desiccator to dry before running in the XRD.

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Running Samples in the D4

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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The D4 Endeavor has several safety issues that should be reviewed. Please see the Bruker Manual D4 Endeavor XRay Diffractometer – Introductory User Manual for the list of precautions.

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Run the NIST 1976 standard (see Quality Assurance/Quality Control) and import the values into the instrument verification spreadsheet. Perform a Zi correction if needed. Calibration of the VANTEC-1 detector may be required. See the detector manual.

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