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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 4C) to the HASKRIS and the water in the tank will begin to cool. The water temperature needs to reach 69°F (Figure 4A). The Haskris temperature can range between 65°F to 69°F (18-21ºC). Ensure all water valves to/from Haskris are open. The flow rate should be greater than 4L/min.

    Figure 4. HASKRIS Control Panel. (A) Actual temperature. (B) Set temperature. (C) On/Off switch. (D) Flow meter

  2. Flip the "ON" switch (Figure 5A) on the side of the Bruker D4 XRD.
    1. The solid green "Low Voltage Ready" light (Figure 5F) turns on.
    2. You will hear several beeps and the "System Ready" light (Figure 5D) will start flashing green.
  3. Press the "High Voltage Enable" button (Figure 5B).
    1. The orange "High Voltage Ready" (Figure 5E) light will turn on.



Figure 5. Side control panel on D4 XRD. (A) Power On/Off. (B) High voltage enable button. (C) Alarm light. (D) System Ready 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 (Figure 6). This enables the mains power and activates the sample handler. 

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  1. Unless the sample material is very small (see Sample Slurry/Smear Slide Mounting for Small Sample Amounts),  select the appropriate sample holder (Figure 8A).
  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 (Figure 8B). Gently press the powder flush with the sample holder using a glass slide (Figure 8C). Roll the glass slide over the powder to fill any gaps in material and smooth the surface of the powder (Figure 8D). The surface of the powder must be smooth. Remove excess powder from the sample holder edges with a brush or a Kimwipe (Figure 8E) and carefully place the holder in the D4 sample magazine .

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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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Regularly check the filter in the HASKRIS tank. If there is a lot of debris it may be necessary to drain the tank and refill with distilled or reverse osmosis (RO) water only - NOT DEIONDeionized. The filter can be sprayed off in a sink taking care not to puncture the screening. If the water flow rate to the system begins to drop close to 4 L/minute it may mean there is a clog in the quick disconnect points behind the back panel or the sprayer head in the X-ray tube housing needs to be cleaned.

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Compare the QAQC corundum scan with past results. X-Ray Tubes deteriorate. When the intensity of the Corundum scan is approximately half of what it was at the date of installation it is time to replace the tube. Check the scans for Tungsten lines, if any appear it is time to replace the X-Ray tube even if the intensity is still acceptable.

Making a Parameter File

A parameter file tells the D4 the conditions that a sample will run under. This is a DQL file made with the XRD Wizard program. The parameter file includes scan settings, scan parameters, generator settings, and beam optics. Some of these settings are constant because they are hardware features of our D4.
To start, double-click the XRD Wizard icon on the Desktop (Figure 33).

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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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