Training and maintenance videos can be found on the XRD technician computer, Desktop/XRD_ICP Prep Documents/Bruker TRAINING VIDEOS
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- 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.
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Figure 4. HASKRIS Control Panel. (A) Actual temperature. (B) Set temperature. (C) On/Off switch. (D) Flow meter
- Flip the "ON" switch (Figure 5A) on the side of the Bruker D4 XRD.
- The solid green "Low Voltage Ready" light (Figure 5F) turns on.
- You will hear several beeps and the "System Ready" light (Figure 5D) will start flashing green.
- Press the "High Voltage Enable" button (Figure 5B).
- 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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- Unless the sample material is very small (see Sample Slurry/Smear Slide Mounting for Small Sample Amounts), select the appropriate sample holder (Figure 8A).
- Label the sample holder with a unique identifier to keep the samples organized (e.g., text ID or 14H2 77-78)
- 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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If X-rays have not been turned on in longer than 24 hours you must turn on tube conditioning to avoid damaging the X-ray tube. In D4 Tools select the icon with the computer and plug. This connects the program to the instrument. Click on the X-RAY generator green button on the status screen, this will show the screen in Figure 31. Or Select "X-RAY" under the Instrument tree. Then select Utilities -> X-Ray Utilities -> Tube Conditioning ON/OFF (Figure 31). The "X-RAY" screen also shows the "Cooling water flow" rate (L/Min) for reference.
Figure 31. D4 Tools X-ray subtree window. (A) X-ray subtree button (B) Utilities command (C) Standing kV and mA
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After about a minute the kV will start to increase in increments from 20kV to 55kV. The whole program takes about one hour and when kV returns to 20 the program is complete. Once this is finished, select the 'Tube Conditioning ON/OFF' again. Note the operational status on the maintenance spreadsheet posted in the lab. To do this click on Manual Control (small head icon) and type GS11. The resulting GS number is the status number. Record this value in the X-ray Tube Conditioning Log.
Turning off the D4 and HASKRIS
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The Beam Optics settings lists the Divergence Slit and AntiScattering Slit (Figure 39). Both of these are constant values based on our hardware setup. The Divergence Slit should be set to .300° (0.6mm). Click "OK" and you will have finished all the settings and will loop back to the first window.
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Figure 39. Beam Optics window.
Save As the file under a new name to the path Local Disk C: > DIFFDAT1. You can print this file by clicking the "Report" tab at the top the subtree window and then clicking the print icon. Occasionally scientists will ask for a printout of the settings to put in their reports.
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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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