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Clay mounts are put onto a zero-background silicon disk that fits into a 2 mm steel sample holder (Figure 2124). Only put the disks into sample holders that have a hole drilled in the bottom. The hole allows the disks to be taken out, otherwise they are stuck inside the holder. The disk should sit flush with the sample holder. Some of the disks are at different depths, so a quartz insert disk can also be put in the bottom of a sample holder with the silicon disk on top. Do not force the zero background disks into the holder, it may break.

Figure 2124: Steel sample holder with silicon disk

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The advantage of the vapor treatment is less disturbance of the sample and less amorphous scattering of X-rays by excess liquid than in the Quick method.

Figure 2225: Glycolator

1. Find the "glycolator" container (Figure 2225) stored in the ICP preparation sink cupboard.
2. Pour ethylene glycol to a depth of ~1 cm in the bottom of the container.
3. Take off the lid and place the samples on the rack inside the glycolator.
4. Place glycolator in an oven (60°–70°C) overnight (~12 hours).
5. Figure 19: Glycolator.Keep samples in the glycolator until ready to run through the D4. Glycolation only lasts for 4 hours after the samples are removed from the glycol atmosphere.

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Open the XRD Commander program using the icon on the toolbar. Figure 2326 is the initial window. Be sure you are in the Adjust tab (btm left, 23C26C).

Figure 2326: XRD Commander main window.(A) Initialize Sample Changer button(B) Initialize Driver Request checkmarks (C) Tabs

First initialize the Sample Changer. The checkmarks (Figure 23B26B) indicate the drives that will be initialized. Check all boxes with values before initializing, click on Init SC (Figure 23A26A). The program then 'locates' all the mechanical drives in the D4. It typically remembers the Theta, 2Theta, and Phi drives but the Divergent Slit sometimes does not initialize. That should not be an issue for scanning samples as our Div. Slit is not mechanical, however if the software won't scan a sample because one or more of the drives did not initialize (successfully initialized drives will turn blue) you can try restarting the program and reinitializing, and/or turning off the D4 and the commander software and restarting the instrument then the commander software and repeating the steps above. If that does not work, close XRD Commander and open D4 Tools from the desktop. Note D4 Tools and XRD Commander cannot be open at the same time.

D4 Tools allows you to see what is causing an error in the D4 instrument and remediate it. In D4 Tools, click "Online Status", then click the icon on the left (Figure ##A27A), this connects the D4 Tools software with the D4 instrument and completes a diagnostics (identifies any errors). The initial diagnostic screen (Figure ##27) shows the instrument status. Any red squares indicates an error. You can investigate the error by clicking on the square. Only trained techs should be trouble shooting errors (errors other than drive initialization) on the D4.  To initialize the drive(s) that did not initialize with the commander software click the '+' positioning drives, then click the drive that did not initialize (Figure ##B28A). Click the Adjust button (Figure ##A28B). 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 (trained in D4 trouble shooting). There is a in-depth sample changer procedure to correct for misalignment in the Bruker Manual (cupboard in XRD lab) but it should only be preformed by trained techs. Alternatively, you can contact Bruker and they can advise or remote into the D4 to fix any errors. Note that some errors can be fixed by clicking the Red Cross icon (Figure ##C28C). The program can identify and fix some errors. Try that icon before contacting Bruker.

Figure ##27: D4 Tools Initial Window. (A) Establishes connection between the software and the D4. (B) Positioning drives select drop down.

Figure ##28. Adjusting a motorized drive via D4 Tools. (A) Select the drive to initialize. (B) Initial Initialize button. (C) First Aid button may help with positioning errors or other errors with the window.

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Click on the Jobs tab (Figure 23C26C). On the Jobs screen, click on "Create Jobs". 

Figure 2429: Create Jobs window. (A) Sample position In D4 sample magazine (B) Sample ID (C) Parameter file (D) Open Directory button (E) Raw file (F) Start button

The window shown in Figure 2429 will pop up. Fill in the Position, Sample ID, Parameter File, and Raw File columns.

• Position: This is the position of the sample in the loading magazine in the D4, from A1–A6 to K1–K6.
• Sample ID: Scan in the label for your sample here. The only format that MegaUploadaTron (MUT) will recognize is Site_Core_Top offset_Bottom offset_TextID (e.g., U1481A_32R4_91_92_QRND8021751). The barcode scanner in the XRD Laboratory is programmed to scan in this exact format including underscores. For special treatments such as clay, glycol or heat treated you must include the treatment in the file name. Add the treatment in the following way U1565A_1R1_3_4_clay_WDGE11053881.
• Parameter File: This is a premade DQL file that sets the conditions under which samples will be scanned. Access the file by clicking on the "Open Directory" button (Figure 24D29D) This directs you to the Control Panel. Follow the path "Local Disk C: > DIFFDAT1. This has a list of all the parameter files from previous expeditions. Select the one that is best suited for your scan parameters.
• Raw File: Sets the location where the results will be saved. Set the location by clicking on the three dots at the end of the cell. Then follow the path "Local Disk C: > DATA > IN". Copy the sample ID into the "Open" line in the window. The sample ID and the name entered into the "IN" Folder must be identical or else the information will not be stored correctly.

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The other fields will automatically populate, you do not need to fill these in and they should not need to be adjusted. Refer to the D4 Commander User Manual for more info on these fields.

Starting a Scan

When all fields have been filled in, click on the "Start" button on the bottom left corner of the screen (Figure 24F29F). The program will hesitate for a moment and then load the first sample into the measurement position and a second sample into the sample changer. The program will automatically run the samples sequentially. If there is an error while scanning the program will stop and notify the user of the error. You can try restarting the software and/or the D4. A sample handler crash may require an experienced D4 XRD tech or you may need to contact Bruker. With the D4 off you can manually move the Z-drive and the sample swing loader, just be aware that the moveable drives are set up to avoid each other during the sample loading sequence, if you move a drive it may cause a crash on start up.

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The RAW file is only readable by the Eva software, whereas the UXD file is a text file that can be read by other programs.
Click the File Exchange software icon on the desktop (Figure 2530).

Figure 2530. File Exchange Desktop Icon

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The initial window (Figure 2631) will open. The left half of the screen is the file input where you select the files you want to convert. The right half of the screen is where you select the new converted file type and where the files should go. 

Figure 2630: First window in File Exchange. (A) Input File Type dropdown menu (B) Input DATA folder (C) Output File Type dropdown menu (D) Output DATA folder (E) Convert button 

First, direct where the new files should be saved and select the converted file type. On the right side, click on the file type dropdown menu (Figure 26C30C) and select "UXD". Then double click on the DATA folder (Figure 26D30D) and direct files to the "IN" Folder.
Move to the left side of the screen and select your input files. Select the file type (Figure 26A30A) "Raw". Click on the DATA folder (Figure 26B30B) and go to the "IN" folder. Here you will see all your samples. Select all the samples and then click the "Convert" button (Figure 26E30E) on the bottom right of the screen. The new UXD files will show up on both sides and you can close down the program.

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Go to the DATA > IN folder where all the sample files are currently stored. Double click on the RAW file and it will open in the Eva software.

Figure 2731. Print Icon

1. Click on the Printer icon at the top of the software outlined in red in Figure 2731. A Print Preview window will open up. On the top bar, click the icon for "Export as a PNG" outlined in red in Figure 2832. This opens the File Save window. Save with the same name as the RAW file. If the names do not match exactly, the files will not upload. Then close the windows and repeat the process for the next sample.
   

Figure 2832: Export Image as PNG Icon

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Before running the NIST standard, carefully remove the anti-air scatter screen. Failure to do this may result in a collision of the drives. The screen is only removed when running the corundum standard to check and adjust system alignment. The anti-air scatter screen should always be on when running samples. (Look in at the video on Desktop/XRD_ICP Prep Documents/Bruker TRAINING VIDEOS to see this done).

1. With two people, carefully remove the cover over the sample staging area, making sure not to hit any wires. The cover is not fastened to the base and will lift off directly.
2. Open D4 Tools and click "Online Status".
3. Click the computer icon to connect with the configuration files in the instrument.
4. Click "Positioning Drives" and "Sample Changer Y" direction.
5. Click "Go", enter "360", and hit "Enter". The sample changer will move in the Y-direction to position 360. This allows you to open the front door and remove the anti-air scatter screen.
6. Open the front door with a socket wrench. Loosen the two bolts on the door and slide the bolts to their opposite side. Carefully let down the door.
7. Remove the anti-air scatter screen (Figure 33). Using an Allen wrench, unscrew the four screws holding up the anti-air scatter screen. These screws are very tiny and easy to drop inside the D4. Be very careful while unscrewing them. The screws are the main support for the screen, so hold onto the screen while removing the screws or else it can fall.
8. When the screws are removed, take off the screen without hitting the theta drives. If the theta drive is knocked, the instrument may signal a hard limit switch error.
9. Close the front door and use the socket wrench to slide the bolts back to their original position and tighten. Go back to the software and move the Y-drive back to Position 1. (Enter "1", "Go", and press "Enter".)

Image ModifiedImage Modified

Figure 33. Anti-air scatter screen in place inside the instrument

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(top image) and after being removed (btm image).

Scanning the NIST 1976 Standard and Verifying QA/QC

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