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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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D4 Tools is a "troubleshooting' software for the D4. T Two other softwares are needed to analyze the diffractograms obtained with the D4.:

• DIFFRAC.SUITE.EVA, version 3.0 software for evaluation (a more recent version, version 5.1, is also available )
  
  
• DIFFRAC.TOPAS version 4.2.0.1 software for diffractogram analysis

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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.
   
   

   

   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 Activity" light (Figure 5D) will start flashing green.
3. Press the "High Voltage Enable" button (Figure 5B).
   1. The "System Activity" light turns green.
   2. An 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 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 (Figure 6). This enables the mains power and activates the sample handler. 

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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),  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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Before beginning measurements, confirm the scan parameters (singles, step and time) with the Science Party. Scientists can use previous Expeditions for examples of ideal scan parameters. Generally the D4 is used to scan from 5 to 70 º2θ. If you need to make a parameter file, please see Making a Parameter File under Maintenance and Troubleshooting. There are several parameter files from previous expeditions saved in the C:/DIFFDAT \DIFFDAT1 folder. Generally a previous expedition file is satisfactory for most expeditions. There are scan variations for Bulk samples versus Clay separations. Those parameter files are labeled accordingly in the DIFFDAT C:\DIFFDAT1 folder. Generally clays are scanned to include much lower angles (<5 º2θ).

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To initialize the drive(s) that did not initialize with the XRD Commander software click the '+' of 'Positioning Drives' to expand the menu, then click the drive that did not initialize (Figure 14A). Click the 'Adjust' button  (Figure 14B). Please note that when you initialize the drives you can hear the drives moving inside the D4. If you hear a clank or bang and the instrument stops working, you will have to get a trained D4 tech. There is a in-depth sample changer procedure to correct for misalignment in the Bruker Manual (in the cupboard in the X-Ray lab) but it should only be preformed by trained techs. Alternatively, you can contact Bruker company and they can advise or remote into the D4 to fix any errors. Note that some errors can be fixed by clicking the 'First Aid' icon (Figure 14C). The program can identify and fix some errors. Try that icon before contacting Bruker company.

Figure 12. Opening D4 Tools.

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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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