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- Unless the sample material is very small, select the appropriate sample holder (see Sample Slurry/Smear Slide Mounting for Small Sample Amounts) (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 (Figure 8) .
Figure 8
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. A. Front-loading sample holders available for the D4. B. Front-loading sample preparation for XRD analysis with the D4
The sample material needs to be flush with the sample holder. The beam is set to focus on the height of the sample holder. If the sample is above or below that focal point, the geometry of the beams do not converge properly, the peak resolution decreases, and the peaks are shifted.
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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).
Figure 9. Back-loading sample holder pieces. A. Sample Ring B. Back piece C. Funneling piece D. Tapper
Figure 10 shows the different steps to prepare back-loading samples.
- Take a front-loading holder and put a clean glass slide over it.
- Take Place the ring, flip it sample ring of the sample holder upside down and put it on the slide (Figure 10)on a glass/plastic plate. Now the powder will fall on a smooth flat surface that will be easy to flip over.
Figure 10. Ring upside down on glass. Funnel piece next to unit.
3. Take the funneling piece and put It inside the ring (Figure 21).
Figure 21. Funnel inside ring.
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- over.
- Place the funneling piece on the top of the sample holder.
- Load the powder into the ring. Try to load the powder evenly across the well.
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- Take the tapping piece and lightly tap down the powder. Use the tool as softly as possible in order to flatten the surface. The idea behind this method is not applying pressure to the measuring face will reduce mineral orientation. Do not tap the powder too firmly or you may unnecessarily orient the minerals.
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- Remove the funneling piece when the powder surface is flat and smooth.
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- Take the back piece and snap it into the ring. Be wary of air displacement.
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- Hold the sample holder and the glass slide. Keep the glass on the sample holder. Flip the whole unit over and set it down.
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Set it down and remove carefully the glass.
The powder needs to be flush with the holder. It may take a few tries to get the right amount of powder in.
Figure 10. Back-loading sample preparation for the D4 sample holders.
Very Small Amount of Material (tooth pick, small crystals, secondary minerals or void filling material)
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In the XRD Commander, click on the 'Jobs' tab (Figure 11C). On the 'Jobs' screen, click on the "Create Jobs" icon 
in the toolbar (Figure 15A).
Figure 15. Create Jobs. (A) 'Create Jobs' icon, (B) Sample position in the D4 sample magazine, (C) Sample ID, (D) Parameter file, (E) Open Directory button, (F) Raw file, (G) Start button
The window shown in Figure 15 will pop up. Fill in the 'Position', 'Sample ID', 'Parameter File', and 'Raw File' columns.********To keep updating from here******
- Position (Figure 15B): This is the position of the sample in the loading magazine in the D4, from A1–A6 to K1–K6. Enter the position manually in the column.
- Sample ID (Figure 15C): 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 X-Ray 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 15E) This directs you to the Control Panel. Follow the path "Local Disk C: > DIFFDAT1 > D4 Bruker ". This folder has a list of all the parameter files from previous expeditions. Select the one that is best suited for your scan parameters.
- Raw File (Figure 15F): Sets the location where the results will be saved. Set the location by clicking on the three dots at the end of the cell (Figure 15G). 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. Click "Open".
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.
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When all fields have been filled in, click on the "Start" button on the bottom left corner of the screen (Figure 29F15H). 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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