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- Haskris water chiller for X-ray tube
- Cahn Model 29 or 31 microbalance
- Mettler-Toledo XS204 dual-balance system
- Powdering equipment:
- Agate mortar and pestle
- Mixer millmills
- Shatterbox
- X-Press
- Glass bottles
- Sonic dismembrator
- Glass rod
- Glass beakers
- Pasteur pipette/eye dropper
- Centrifuge and centrifuge tubes
- Desiccator
- Labconco Freeze Dryer
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Retsch MM400 Mixer Mill
The manufacturers manufacturer's manual for the Retsch MM400 can be found here (XRD Lab Notebook).
Figure 16: Retsch MM400
Figure 17. Agate grinding jars and ball.
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Each grinding jar has the main jar, the lid and ball, and the white teflon spacer. Use the spacer to avoid damaging the agate. The inside of the jar and lid are lined with agate and the ball of made of agate. Poor freeze dried soft sediment (not hard rock) sediment grains into the jar. Fill the jar half way to three-fourths of the way up with sample. Place one (can do take two) grinding balls in the jar. Clean off any of the sediment sample with a kimwipe that has gotten onto the jars threads and screw the lid on. Be mindful not to cross thread the lid to the jar.
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After grinding jars are secured in clamps, the pin is in the closed position and the clear cover is closed it is time to select grinding settings. Program 1 (A) is currently set for 12 min at 25 1/s. This setting is good for clay rich material. Softer sediments such as CaCO3 typically need less time. It is important to only grind soft sediments in the agate jars and hard material should be ground in the shatter box. After Grinding cycle has completed twist completed turn knob counter clockwise and pill pull pin up and into its open position (Figure 18a). Unscrew clamp and open jar to verify grind size. If sediment is still too coarse regrind.
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After grinding is complete remove grinding jar from clamps. rotate black screw counter clockwise a quarter turn and pull the pin up into the open position (Figure 18a). open When the pin is in the open position unscrew black knob until grinding gar is loose enough to remove. Unscrew grinding jar, poor powder onto weigh paper or directly into clean and labeled sample bag.
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To clean the jars amd grinding ball rinse with DI water and kim wipes until kimwhipes come out clean. Finish cleaning by rinsing with isopropal alcohol and drying with kim wipe. Use the bent metal spatula to pry out the white teflon spacer, we have spares but these those can be reused many times.
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9. Remove 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.
Very Small Amount of Material (tooth pick, small crystals, secondary minerals or void filling material)
Sample Slurry/Smear Slide Mounting for Small Sample Amounts
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Before beginning this procedure, confirm the scan parameters (singles, step and time) with the Science Party. Scientists can use previous Expeditions for examples of ideal scan parameters. Generally the D4 is used to scan from 3 5 to 70 x 2Theta. If you need to make a parameter file, please reference Making a Parameter File under Maintenance and Troubleshooting. There are several parameter files from previous expeditions saved in the C:/DIFFDAT folder. Generally a previous expedition file is satisfactory for most expeditions. There are scan variations for Bulk samples versus Clay separations. Those parameter files are labeled accordingly in the DIFFDAT folder. Generally clays are scanned to include much lower angles (<5 deg 2Theta).
Open the XRD Commander program using the icon on the toolbar. Figure 23 is the initial window. Be sure you are in the Adjust tab (btm left, 23A).
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First initialize the Sample Changer by clicking on Init SC (Figure 23A). The checkmarks (Figure 23B) indicate the drives that will be initialized. Check the "Div. Slit" box before initializing; the program all boxes before initializing, click on Init SC (Figure 23A). The program then 'locates' all the mechanical drives in the D4. It typically remembers the Theta, 2Theta, and Phi drives . Successfully initialized drives will turn blue. If one or more stay red, 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 following 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. Click the icon on the left (Figure ##A), this connects the D4 Tools 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 ##). 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.
Go to the drives that will not initialize and click the "Adjust" button. Then close D4 Tools and reopen XRD Commander. The "Adjust" command can also initialize the drives. The diffractometer's sample-changer drives will adjust inside the instrument. If you hear a crash or the program gives an error, see the procedure for readjusting the sample handler in the Bruker manual. This is a lengthy process.
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