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Figure 21. Small vessel filled with sample pieces. No sample material is on the top the puck or in the lid ring.
Figure 22. The inside of the Shatterbox.
A. The lever arm B. The clamp arm C. The inner capsule Open the lid, pull out the lever arm (Fig. 22A), and pull up the clamp arm (Fig. 22B). This will reveal full access to the inner capsule (Fig. 22C).
Figure 2322. Inside the Shatterbox with the bottom three pinned rack plate resting inside the inner capsule.Depending The inside of the Shatterbox. A. The lever arm B. The clamp arm C. The inner capsule
Depending on vessel size, you will either put in the pinned plate (small vessels) or the large vessel directly. The shatterbox setup will also vary depending on sample number. If you are crushing one sample use the one pinned plate, whereas for two or three samples use the three pinned plate (Fig. 23). For crushing two samples, two vessels will be full, whereas the third will be empty without a puck. It is important to maintain balance within the machine to prevent damage.
Figure 23. Inside the Shatterbox with the bottom three pinned rack plate resting inside the inner capsule.
Now load vessels onto the plate (Fig. 24). The divet in the bottom of the vessels will settle onto the pins and fit firmly in place.
Figure 24. Three samples loaded into the Shatterbox.
Put the top rack plate over the vessels. Bring down the clamp arm (Fig. 25A). The guide on the clamp arm will settle into the boss (Fig. 25B) when centered properly. Bring the lever arm down and push it into the end of the clamp arm (Fig. 26B). Then push the lever arm down over the clamp arm (Fig. 26A
).
Figure 25. The top rack plate sitting on top of the three samples. A. Clamp arm. B. the "boss" “boss” of the rack plate, where the clamp arm will attach.Figure 24
Bring the lever arm down and push it into the end of the clamp arm (Fig. 26B). Then push the lever arm down over the clamp arm (Fig. 26A).
. Three samples loaded into the Shatterbox. 
Figure 26. A. The lever arm inserted into the end of the clamp arm. B. The clamp arm pushed over the lever arm.
The resistance in the lever arm is very important and must be adjusted before use. There should be moderate resistance in the arm while pushing it down. If the resistance is too low the containers can shake free; whereas, if it's too strong the clamp can break. Ideal tightness is just past the point where the vessels can be rotated while the clamp is down. Adjust the resistance by raising the clamp arm and pushing on the 'locking pin.' Hold the locking pin and turn the guide (Fig. 27A). Rotating the guide clockwise decreases resistance; whereas counterclockwise increases resistance.
Figure 27. The lever arm and the guide. A. Retractable locking pin being pushed to allow adjustment of the 'guide' length.
Now close the lid and turn the emergency stop switch to 'On'. This does not start the Shatterbox but does enable operation. If an emergency shutdown is needed, flip this switch to 'Off' and all shaking will stop even though the timer will continue to count down.
Set the grinding time. The LCD screen displays the current operating time (Fig. 28A). Adjust the time by pressing on the 'Minute' (Fig. 28B) and 'Second' (Fig. 28C) buttons. The timer maximum is 9:59.
Figure 28. A. Current operating time. B. Minute button. C. Second button. D. Start button. E. Pause/Stop button.
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Disassemble the vessel carefully wearing 'Powderless Nitrile' gloves. Clean off any powder on the lid or puck with clean gloves or a kim wipe. Carefully remove the puck from the vessel. Pour the sample onto a clean weighing paper. If any powder remains, use a clean plastic spatula, brush, or your finger to dislodge it.
Note: Never use metal to dislodge sample material, as any grooves or scratches in the vessels will increase the risk of contamination.
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Cleaning the Grinding Vessels
Vessels must be cleaned in between samples and after all samples have been run for the day. Vessels should never be put away wet. This alters and tarnishes the vessel.
In Between Sample Runs
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After the last run for the day
1. Take a scoop of quartz sand and put it in your vessel and run it as you would a sample for several minutes.
2. Remove the vessel and empty out the sand. Scrub the pieces with DI water and a scouring pad. Then spray with isopropyl alcohol and wipe down with Kim Wipe.
If your vessel is particularly dirty run a combination of quartz sand, a little hot water and detergent (Borax). This can be run for several minutes. A thick paste will form and you clean it with DI water and isopropyl as in the other cases.
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Making the Sample Bead
Two processes are required to make a sample bead:
- In a vial, mix 400 mg lithium metaborate flux (pre-weighed onshore) with non-ignited, or raw, powdered sample. This step is typically completed by the chemistry technicians.
- Fuse both sample powder and flux into a glass bead (Fig. 4429). Dissolve the bead in nitric acid. This solution will be further diluted and analyzed by the ICP.
Figure 4429. Fused glass bead. 
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Weighing the Sample
Note: This process is typically done by the chemistry technicians.
Weighing the ignited sample is a critical step. The sample weight should be as close to 100 mg as possible. Inaccuracies in the weight will show up in the analytical results. Print small labels for each sample and place on your small, clear capped vial. On the lid label a sticker with the core, section, and interval.
- Clean the countertop around the balance and the balance pans with isopropyl alcohol. Put sheets of white paper on all the working surfaces.
- Arrange all supplies on the white paper: tweezers, scoopula, and a sheet of 6x6 weigh paper.
- Ensure the following items are available and labeled for each sample.
- 1 bottle of pre-weighed flux
- 1 new, empty, acid-washed vial for the remaining ignited powder
- Pre-label the bottles before weighing (one label each on the cap and the bottle).
- Make two weigh boats. Cut a rectangular strip from your piece of weigh paper and fold up the two long sides. Put one on the 'Tare' Side and the other on the sample side. You will need to make a new boat for each sample. The tare boat will remain there for all of your samples.
- Close the door of the balance and tare for 100 counts.
- Remove a crucible of ignited powder from the desiccator. If the powder has hardened from the furnace then transfer the sample from the crucible to a clean agate mortar and grind until it is a loose fine powder. If your sample is fine proceed to the next step.
- Keep your boat in the weigh pan and with your scoopula measure out 100 grams. Be careful not to spill your sample onto the pan. If you do remove your sample boat and with a small brush wipe away the loose powder.
- Close the door and weigh the sample, putting more sample on or off until you achieve a reproducible weight that is within ±0.00050 g of 0 (half a milligram).
- When the sample weight is as close to 100 mg as you can get it (i.e., 0.0995–0.1005 g), open the labeled bottle with the pre-weighed flux and carefully pick up the paper with the sample powder on it and transfer all of the powder into the bottle containing the flux. Snap the paper a few times with a flick of your index finger to make sure everything goes in.
- Homogenize the sample/flux mixture by holding the vial slightly off of vertical and rotating it. Tap it from time to time on the bench top as you rotate it to clear any powder from the sides of the vial. Avoid getting the sample/flux powder stuck around the cap.
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Fusing the Sample into a Bead
The most critical aspect of bead-making is maintaining a constant sample to flux ratio. A ratio of 1:4 suffices in most situations. If samples are small (e.g., volcanic glasses), a sample mass <0.1 g may be used. However, the same ratio must be maintained between the samples and the calibration standards (otherwise the matrix will not match). For example, 0.05 g of sample requires 0.2 g flux.
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Using the Beadmaker
Collect platinum crucibles, platinum tipped tongs, 0.172 LiBr, and pipette tips from the safe above the Bead Maker. Get the 10-100ul pipette and teflon spatula from the drawer and clean with isopropyl alcohol. Have a tray of samples that need to be fused and an empty tray for finished beads.
Figure 4530. Bead making supplies. A. Platinum tipped tongs. B. Platinum crucibles. C. 0.172 Libr wetting agent. D. Pipette. E. Teflon spatula. F. Pipette tips.
Figure 46. Bead making supplies. A. control panel. B. Site of platinum crucible. C. View port window. D. Fan to cool platinum crucible. E. Ceramic plate used for dislodging the fused bead.
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