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.
Two other softwares software applications 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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- 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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7. If this is the first time in 24 or more hours than 4 days that the D4 has been turned on, the X-ray tube needs to be conditioned. Go to the Maintenance section under Tube Conditioning for instructions and log the date of tube conditioning in the XRD maintenance log in XRD's Lab Notebook on Confluence.
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The Bruker D4 can be kept on when not in use. However during extended periods such as Tie-ups or if there is not someone to check on the instrument it can be shut down. The Haskris can also remain on, or it can be turned off if no one is able to monitor it. If the Bruker D4 is on, the Haskris must be on as well. 1.
- Turn the X-Ray generator off by turning the key counterclockwise (Figure 6).
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- Push the Red mains button (Figure 6).
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- Turn off the High Voltage button B as shown in Figure 5.
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- Turn off the
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- detector button A as shown in Figure 5.
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NOTE: Sample Preparation for XRD Analyses is in the main Laboratory Manuals, Guides and Resources>XRD confluence page.
Sample preparations are preparation is split into two 3 main categories:A. Bulk powder samples
B. Clay separations
- Bulk Sediment
- Hard Rock
- Clay Separation
Before running samples, go over the methods with scientists and check for any special sample requests.
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Make sure the sample from the sampling table (in the Core lab) is enough material to fill a sample holder - sample size for bulk powder is generally a 1-2 cm QRND (Quarter Round) from the section half. This will produce more than enough material to fill a sample holder. You do not want more than this as it will be wasted.
Front-Load Samples
This technique is commonly used to prepare samples to be measured with the D4.
- 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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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 as a low broad peak at ~7.3º 2θ in the diffractogram.
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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 4 days you must turn on complete a cycle of 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.
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After about a minute the kV will start to increase in increments from 20kV to 55kV. The whole program cycle takes about one hour and when the kV returns to 20 the program cycle is complete. Once this is finished, select the 'Tube Conditioning ON/OFF' again. Note the operational status on the maintenance spreadsheet posted in the labin the 'Preventative Maintenance' page of the X-Ray Lab Notebook on Confluence. To do this click on Manual Control (small head icon) in D4 Tools and type GS11. The resulting GS number is the status number. Record this value in the X-ray Tube Conditioning Log.
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First turn off the D4 in the opposite order that you turned it on: Turn the key to off, turn off push the red mains power button, disengage depress the high voltage button on the left side of the Bruker, and then turn off the power switch also on the left side. The Haskris chiller must remain running for at least one hour after turning off everything else the XRD to properly cool down the X-ray tube. The D4 can be off while leaving the chill water on, but if the HASKRIS is off the D4 must be off.
Cleaning the Diffraction System
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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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