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The follow instructions are for two mixer mills, Spex 8000 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.
Figure 98: Spex 8000 mixer mill. Featured are the safety latch, timer dial, and start/stop button in the middle of the dial.
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There are three types of grinding vessels available for the 8000 mixer mill: alumina ceramic, tungsten carbide, and hardened steel (Figure 119). 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.
Figure 119: Three types of mixer mill grinding vessels.
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Below are the components for each type of vessel. The steel (Figure 1210) and tungsten carbide (Figure 1311) both have a vessel body with attached lid and one separate lid that is screwed on. Cross-threading is very easy with these containers, so be very careful when screwing on the lid. Also note that the steel container has an O-ring, whereas the tungsten carbide does not. The alumina ceramic vessel (Figure 1412) is assembled differently than the other two vessels: two cork rings are placed inside each lid, and the lids slip onto either side of the vessel body. 
Figure 1210: Steel vessel components. (A) Lid (B) Container (C) Steel Grinding Ball (D) O-Ring
Figure 1311: Tungsten carbide vessel. (A) Vessel container (B) Lid (C) Tungsten carbide grinding ball
Figure 1412: Alumina ceramic vessel components. (A) 2 cork rings (B) Vessel body (C) Alumina ceramic grinding ball (D) 2 lids
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Put your sample inside the vessel. The material should be approximately the size of a pea to prevent any jamming and to ensure all pieces are ground up. Place 1 to 2 grinding balls inside the container. Tungsten carbide and steel vessels can take up to 2 balls. The alumina ceramic vessel is more brittle and 1 ball is recommended. Finish assembling the grinding vessel and open the lid to the mixer mill.
Figure 1513: Inside the 8000M mixer mill. Highlighted is the sample holder clamp that holds the grinding vessels, the primary lock, and the secondary lock.
Hold the grinding vessel between the sample holder clamps (Figure 1513), flush against one side. Still holding the vessel, start turning the primary lock. The holder will begin to clamp down on the sample. When the vessel is secured, you can remove your hand and continue tightening the primary lock until the sample is firmly gripped. Then tighten the secondary lock until it feels firm. Check the vessel to make sure the lids are resting flat on the clamps. If the vessel is ajar inside the clamp, when the motor starts the vessel can start grinding away at itself or fly loose into the machine.
Starting the Mill
Set the timer to the desired grinding time. The time will vary depending on sample material. Start with a conservative time, 2 to 3 minutes, check the material, and add more time if the sample still feels gritty. Harder rocks can go up to 10 minutes or beyond higher to grind down to the right sample consistency.
When When the mill finishes grinding, remove the vessel the same way as it was put into the clamp: hold the vessel firmly against one clamp while unscrewing the primary lock. Keep the vessel straight and hold it firmly. If one of the lids starts to crack open, sample material will spill into the machine. If this happens, clean up the powder with a damp towel. Any leftover powder can get into the motor and damage it.
Transferring Powder
Collect a metal tray, weigh paper (large or small), 8 or 16 mL clear snap cap bottles, a scoopula, Kim Wipes, and isopropyl alcohol. Clean all materials with isopropyl alcohol. Place a piece of weigh paper on the metal tray. Pour the sample material from the grinding vessel onto the weigh weighing paper. Use the scoopula to scrape the sides and lids of the vessel to remove extra material. Transfer the sample from the weigh weighing paper into the glass sample vial. Label the vial with a small printed label and label the cap with a permanent marker.
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 (can be trashed in burnables or collected and thrown overboard) and clean the vessel with DI water and a toothbrush or Greenie Meaniegreen scrub pad. 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 Mixer Mill
The manufacturer's manual for the Retsch MM400 can be found here (in Retsch MM400 XRD Lab Notebook). Figure 14 shows the Retsch mixer mill.
Figure 1614: Retsch MM400
Figure 1715. Agate grinding jars and ball.
Each grinding jar has the for the Retsch mill (Figure 15) has a main jar, the a lid and , a ball, and the white a white teflon spacer. Use the spacer to avoid damaging the agate (Figure 16). The inside of the jar and lid are lined with agate and the ball is of made of agate. Poor the 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 take two) grinding balls ball 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.
Figure ##16. Agate grinding jars with teflon spacer and the bent metal spatula for removing the teflon spacer.
Loading the Jar into the Grinding Mill
Place closed grinding jar horizontally in the clamps. Verify the pin is in closed position (Figure 17) and tighten the clamps by turning the handle until the jar is securely tighten (hand tight is good). Close lid and select desired program to run.
Figure 18 MM400 Grinding 17. Retsch jar clamp
Starting the Mill
After the grinding jars are secured in the clamps, the pin is in the closed position and the clear cover is closed it is time to select grinding settings (Figure 19). 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 turn knob counter clockwise and pull pin up and into its open position (Figure 18a19A). Unscrew clamp and open jar to verify grind size. If sediment is still too coarse regrind.
Figure 19 18 A) Preset programs. B) The shaker frequency C) The time grinder is set for D) The start and stop.
Transferring Powder
After grinding is complete remove grinding jar from clamps. rotate Rotate black screw counter clockwise a quarter turn and pull the pin up into the open position (Figure 18a17). 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 or sample vial.
Cleaning the Jars
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 those can be reused many times.
Shatterbox
Shatterbox vessels are not commonly used for powder sediment XRD samples. Please refer to the XRD Sample prep for hard rock samples for instructions for using the shatterbox.
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