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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).
- 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. Gently press the powder flush with the sample holder using a glass slide. Roll the glass slide over the powder to fill any gaps in material and smooth the surface of the powder. The surface of the powder must be smooth. Remove excess powder from the sample holder edges and carefully place the holder in the D4 sample magazine.
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D4 Tools allows you to see what is causing an error in the D4 instrument and remediate it. In D4 Tools, click the icon on the left (Figure ##A), this connects the D4 Tools software with the D4 instrument and completes a diagnostics (identifies any errors). The initial screen (Figure ##) 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 ##B). Click the Adjust button (Figure ##A). 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 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 ##C). The program can identify and fix some errors. Try that icon before contacting Bruker.
Figure ##: D4 Tools Initial Window. (A) Establishes connection between the software and the D4. (B) Positioning drives select drop down.
Figure ##. Adjusting a motorized drive via D4 Tools. (A) Select the drive to initialize. (B) Initial button. (C) First Aid button may help with positioning errors or other errors with the window.
Entering Sample info into the Commander
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- 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.
- 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 24D) This directs you to the Control Panel. Follow the path "Local Disk C: > DIFFDAT1 > DIFFDAT1_old computer pre March 2013". 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. These , you do not need to fill these in and they should not need to be adjusted. Only change the other settings if you know what to do and refer to Refer to the D4 Commander User Manual for info on these fields.
Starting a Scan
When all fields have been filled in for all samples, click on the "Start" button on the bottom left corner of the screen (Figure 24F). 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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