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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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There are 10 back-loading holders. The holder has an empty ring (Figure 9A) and backing piece (Figure 9B) that snaps in from behind. There are also two loading pieces. One piece helps funnel the powder (Figure 9C) in and the other taps down the powder into a flat surface (Figure 9D). Note: If the layer of sample is not think enough or the sample is composed mostly of very light elements (such as freeze-dried calcareous ooze), the sample holder material (PMMA plastic) will show a low broad peak at ~7.3º 2θ in the diffractogram.

Figure 9. Back-loading sample holder pieces. A. Sample Ring B. Back piece C. Funneling piece D. Tapper

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The .RAW file is not readable for most other software, whereas the .UXD file is a text file that can be read by other programs. Therefore, we upload both of files types to LIMS. DIFFRAC.Eva can open/import .raw and .xy files, whereas HighScore Plus (available to the scientists via a virtual computer, see HighScore Software Plus Quick Start Guide) can open .raw, uxd, .xrdml, and .xy XRD file types. See the Aeris Advanced user Guide for instructions on converting .xrdml (Aeris) files to .xy.
To convert a .RAW file to an .UXD file, click the Diffrac.File Exchange software icon on the desktop (Figure 16).

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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 DI distilled or reverse osmosis (RO) water only - NOT DEION. 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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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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