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7. If this is the first time in 24 (is this correct?) 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.
Shutting Down Bruker D4
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The Bruker D4 can be kept on when not in use. However during extended periods such as Tie-ups or if there is not someone to check on the instrument it can be shut down. The haskris can also remain on, or it can be turned off if no one is able to monitor it. If the Bruker D4 is on the Haskris must be on as well.
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NOTE: Sample preparation is discussed in more detail under Sample Prep in the main XRD Manuals confluence page.
Sample preparations are split into two main categories:
A. Bulk powder samples
B. Clay separations
Before running samples, go over the methods with scientists and check for any special sample requests.
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Pour sample into the mortar and grind the sample with the pestle. When finished, the sample should be the consistency of talc powder. Test the sample by taking a pinch and rubbing it on your skin. If the sample feels gritty, it needs to be ground more. If the texture is good and the sample looks homogenous, you can pack the sample into a sample holder to be placed in the D4.
Mixer millMills
The The follow instructions are for two mixer mills. Currentlythe Retsch400 , Spex and the Newer Retsch MM400. Currently the Retsch MM400 is the recommended mixer mill to use and it is located in X-Ray Prep or MBIO area of Chem lab. There are two mixer mills located in X-Ray Prep. Both mills operate very similarly but do have slight differences (Figure 9; Figure 10).
Figure 9: 8000 mixer mill. An older simplified version of the 8000M. Featured are the safety latch, timer dial, and start/stop button in the middle of the dial.
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To operate the 8000 mixer mill, turn the knob to the desired time and press the "Start" button in the middle. That button will also stop the mixer mill. The dial does not move automatically, so if it is turned to 5 minutes it will stay there. The dial does not need be set back to 0 to work.
Grinding Vessels
There are three types of grinding vessels available for the 8000M 8000 mixer mill: alumina ceramic, tungsten carbide, and hardened steel (Figure 11). Tungsten carbide and steel vessels are better for more robust grinding, and alumina ceramic is better for minimizing contamination. Check with the Science Party to see which vessel type is preferred.
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Cleaning the Vessels
Clean the grinding vessels with a toothbrush and DI water. In some cases the vials are still dirty or have sample stains on them. If so, take a small amount, approximately 5 mL, of silica sand and grind it in the mixer mill for ~3 minutes. Then pour out the sand and clean the vessel with DI water and a toothbrush or Greenie Meanie. Lay out cleaned vessel parts on a Kim Towel and dry with a Kim Wipe. The cork rings take a longer to dry, so collect fresh, dry rings before grinding the next sample.
Then can now pack the samples.
Retsch MM400
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Mixer Mill
The manufacturers 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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