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The instruments in the lab need to be turned on in this order: (1) HASKRIS and (2) D4 XRD. The HASKRIS cools the water supplied to the D4 to prevent the X-ray tube from overheating. Turning the D4 on prematurely will could damage the X-ray tube.
Procedure for Turning on Instruments
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- Flip the "On" switch (Figure 1C) to the HASKRIS and the water in the tank will begin to cool. The water temperature needs to reach 69°F (Figure 1A). The Haskris temperature can range between 65°F to 69°F. Ensure all water valves to/from has kris haskris are open.
Figure 1. HASKRIS Control Panel. (A) Actual temperature. (B) Set temperature. (C) On/Off switch. (D) Flow meter
- Flip the ON switch (Figure 2A) on the side of the machine.
- The solid green "Low Voltage Ready" light (Figure 2F) turns on.
- You will hear several beeps and the "System Activity" light (Figure 2D) will start flashing green.
- Press the "High Voltage Enable" button (Figure 2B).
- The "System Activity" light turns green.
- An orange "High Voltage Ready" (Figure 2E) light will turn on.
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Figure 2. Side control panel on D4 XRD. (A) Power On/Off. (B) High voltage enable button. (C) Alarm light. (D) System activity flashing light. (E) High voltage ready light. (F) Low voltage ready light.
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4. Go to the front of the machine and press the green circular button. This enables the mains power and activates the sample handler (see Figure 34). 
Figure 3. D4 top Front control lightspanel.
5. Turn the “Generator Power” key to the right for a few seconds and look at the lights on top of the D4 (Figure 4)
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When the “Alarm” light turns off and the “Ready” light turns on, release the key back into its middle position.
Figure 4. D4 top control lights.
6. The top of the machine should have a solid orange “Ready” light and a solid green “On” light.
7. If this is the first time in 24 (is this correct?) or 24 or more hours that the D4 has been turned on, the X-ray tube now needs to be conditioned. Go to the Maintenance section under Tube Conditioning for instructions and log the date of tube conditioning in the XRD maintenance log in XRD's Lab Notebook on confluence.
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Mortar and pestle is the most common method for sediment. Below, each method is outlined. Any sample material remaining once all analyses are complete 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 at End of Expedition, or when all possible rescans and special treatments are completed.
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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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- Cut open the sealed sample bags and fold the top edge over to keep the bag open.
- Take the top of the bell off of the dryer and arrange samples in the bell, making sure no sample bags are pinched closed.
- Close Open the vacuum valves slowly so that you do not cause a large rush of air to blow the samples around. Figure 5A shows the configuration to dry samples and Figure 5B shows the configuration for loading and unloading samples.
- Set the freeze dryer to resemble the settings shown in Figure 6 and flip the Flip the "On" switch located on the right side of the machineFreeze Dryer.
- Press the "Auto Refrigeration" button (Figure 6A) and then the vacuum button (Figure 6B). The temperature will start to drop and the vacuum pump will turn on.
- When the temperature drops to –40°C, the vacuum is created in the bell and the pressure drops.
- Expect the temperature to be between –42° and –52°C and the pressure to be ~0.350 mBar.
- The indicator lights (Figure 6D) show how the cooling and pressure reduction are progressing. When all indicator are lights are on the freeze dryer is at its peak performance.
- If there is an error the red "Alarm" light will turn on. Press the "Menu" button (Figure 6C) to view it and clear it if necessary.
- After samples are dry, slowly open the valves to let out release the vacuum in the bell. Remove the samples from the bell and store them inside the desiccator until they are ready to be ground to prevent reabsorption of moisture.
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