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Mortar and pestle is the most common method. Below, each method is outlined. Any sample material left in the sample bag can be given to the Curator at the end of the expedition to be sent back to the repository. Any sample that has been treated should be disposed of when measurements are completed. However, samples should be kept for a couple weeks after scanning in the XRD as some samples may be scanned again or have multiple treatments.
Drying Samples
Freeze-dry sample(s) for at least 12 hours before grinding. If the samples still feel cold when removed from the dryer, the samples still have moisture in them and need to dry longer.
The freeze dryer is comprised of a sample "bell" chamber and a Labconco freeze-dryer. On the bell are two valves, as shown in Figure 5. Each valve has an "Open" and "Closed" position. The top valve controls the vacuum inside of the bell, and the bottom valve controls the air flow between the cooling coil and bell. A valve parallel with the tube is open and allows air flow; a valve perpendicular with the tube is closed. In Figure 5, configuration A (closed) will hold a vacuum, but configuration B (open) will not.
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- When the muffle furnace has finished its program heating and is cooling down, wait until the temperature reaches between 100° and 200°C before removing the sample. The sample can be placed in the desiccator until it reaches room temperature. Once it has completely cooled down it can be run in the D4.
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Before beginning this procedure, discuss confirm the desired scan parameters (singles, step and time) with the Science Party. 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 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.
Open the XRD Commander program using the icon on the toolbar. Figure 23 is the initial window.
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