Before being crushed in the X-Press, hard rock samples for ICP analysis are polished (Figure 1.1 and 1.2) and cleaned in a sonic bath at least three times (for 10-15 minutes each): the first round of cleaning is with isopropyl alcohol and the following rounds are with DI water (Figure 1.3, see ICP Preparation for further details). Hard rock samples for XRD analysis do not usually need to be polished before being crushed.
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After the sample has cracked, release the toggle switch. To remove the unit, loosen the pressure relief handle (Figure 4A, arrow C) by rotating it counter clock wise and press hold down on the toggle switch. The pressure gauge should read zero and the metal platform will lower down. Do not leave the platform up, always make sure to lower it back down after crushing a sample. When the platform is level with the surface let go of the toggle switch and start unscrewing unscrew the jackscrew. Then open slide the polycarbonate door up and remove the unit. The pieces can be poured into a labeled bottle that will eventually hold the finely ground powder. From here the pieces will then be put into the Shatterbox vessels.
If pieces are still too large then repeat the same setup and crush it again. Look out for and remove any pieces of the Delrin Discs that may have chipped off and gotten into the sample. Leaving pieces of the Delrin Discs in the sample will cause contamination.
It may happen that the metal platform does not lower down completely after the pressure releaseis released. In that case, remove the crushing unit and replace it by the aluminum cylinder (Figure 5). Leave the " pressure relief handle " loose. Tighten the aluminum cylinder with the jackscrew. Close Slide the door in place and press down the toggle switch. Rotate the jackscrew to keep the aluminum cylinder tightened as pressure increases and the platform lowers down. When the platform is level with the surface, let go of the toggle and unscrew the jackscrew. Remove the aluminum cylinder and proceed to the next sample.
Figure 5. How to lower down the metal platform.
Grinding Samples in the Shatterbox
The shatterbox takes the crushed pieces from the X-Press and grinds them into a very fine powder. The Spex shatterbox is capable of grinding three standard size samples or one large sample. Our We use tungsten carbide grinding vessels used are tungsten carbide.
Apparatus and Materials
- Shatterbox
- Tungsten Carbide Vessels: Vessel, Puck, and Lid
- Samples
- 1oz Sample Vials
- Sample Labels
- Teflon spatula
- Weigh paper 6" x 6"
Turn on the Shatterbox by flipping the 'On' switch located on the back panel (Figure 6A6A, arrow A). The control panel (Figure 6B6B) is located on the front of the lid (Figure 6A6A, arrow B) next to the handle.
Figure 6. A. Shatterbox. A. Power switch. B. Control panel. C. Emergency Stop switch. B. Control Panel
There are two sizes of grinding vessels: small and large. Each size has different components and requires a different setup inside the Shatterbox. The small vessel holds between 5-20 mL of material and has three components: container, puck and lid (Figure 7). The small vessels are usually used for grinding samples for ICP analysis.
Figure 7. Small vessel components. A. Container B. Puck. C. Lid
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The three-pinned plate will hold three grinding vessels while the one-pinned plate will only hold one . If two samples need to be crushed select the three-pinned plate and add sand in a third vessel to maintain balance in the shatterboxgrinding vessel.
The large grinding vessel will sit directly in the shatterbox without an additional plate below it.
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Transfer the sample pieces into the grinding vessel. Pour sample pieces between the puck and the wall of the vessel (Figure 11). There can't be any material on top of the puck or inside the sealing ring; otherwise the vessel will on top of the walls of the container (the area the lid sits on); otherwise the vessel will not seal properly and the sample can spill inside the shatterbox. If any pieces are on top of the puck or ring, use gloves, tongs, or a KimWipe to move the sample into the vessel. Put on the lid and start assembling the shatterbox.
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Open the lid, pull out the lever arm (Figure 12, arrow A), and pull up the clamp arm (Figure 12, arrow B). This will reveal allow full access to the inner capsule platform (Figure 12, arrow C).
Figure 12. The inside of the Shatterbox. A. The lever arm B. The clamp arm C. The inner capsule platform
Depending on vessel size, you will either put in the one- or three- pinned plate (small vessels) or the single large grinding vessel directly. The shatterbox setup will also vary depending on sample number. If you are crushing one small sample, use the one-pinned plate with one small grinding vessel, whereas for two or three samples use the three-pinned plate (Figure 13). For crushing two samples, two vessels will be full with sample, whereas the third will be empty without a puck or you can add container can have quartz sand added to the third containerit. It is important to maintain balance within the machine to prevent damage.
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Figure 13. Inside the Shatterbox with the bottom three-pinned rack plate resting inside the inner capsule.
Now load vessels onto the plate (Figure 14). The divet in the bottom of the vessels will settle onto the pins and fit firmly in place.
Figure 14. Three samples loaded into the Shatterbox.
Put the top rack plate over the vessels. Bring down the clamp arm (Figure 15, arrow A). The guide on the clamp arm will settle into the boss (Figure 15, arrow B) when centered properly.
Figure 15. The top rack plate sitting on top of the three samples. A. Clamp arm. B. the “boss” boss of the rack top plate, where the clamp arm will attach.
Bring the lever arm down and push it into over the end of the clamp arm (Figure 1616A, arrow B). Then push the lever arm down over the end of the clamp arm (Figure 16, arrow A16B).
Figure 16. 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 each use. There should be moderate resistance in the lever arm while pushing it over and down onto the clamp arm. 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.' ' on the clamp arm (Figure 17, box). Hold the locking pin and turn the wheel guide (Figure 17, double headed arrow A). ) to loosen or tighten the pressure of the clamp on the containers. Rotating the guide clockwise decreases resistancetightens; whereas counterclockwise increases resistanceloosens.
Figure 17. The lever arm and the guide. A. Retractable locking pin being pushed to allow adjustment of the 'guide' length.
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and the wheel guide.
Now close the lid and set the grinding time. The LCD screen displays the current operating time (Figure 18, arrow A). Adjust the time by pressing on the 'Minute' (Figure 18, arrow B) and 'Second' (Figure 18, arrow C) buttons. The timer maximum is 9:59. 
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When the time is set press the 'Start' button (Figure
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6B). To temporarily pause the operation press the 'Pause
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' button
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. The machine will stop, but the lid will not unlock. To stop the machine press '
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Stop'
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and when it has slowed enough, you will hear the click of the lid unlocking.
Normal Sounds: The shatterbox is extremely loud. The foam and strap surrounding the shatterbox helps keep it in place and minimize some of the noise.
Abnormal Sounds. If there are any metal on metal sounds shut off the shatterbox immediately. Something inside the shatterbox has probably come loose and will damage the inside of the container.
When the shatterbox cycle is done open the lid and remove the vessels, placing them on the counter. Open the grinding vessel and with clean tweezers take a bit of the powder and feel it against the inside of your wrist. The sample should feel like baby powder, if it does not, repeat the shatterbox cycle. A 1 to -3 min minute cycle is enough for most of rocks.
Transfer powder into Vial
Disassemble the vessel carefully wearing 'Powderless Nitrile ' gloves. Clean off any powder on the lid or puck with clean gloves or a Kim Wipeteflon spatula. Carefully remove the puck from the vessel. Pour the sample onto a clean weighing paper. If any powder remains, use a clean plastic teflon spatula, brush, or your finger to dislodge it.
Note: Never use metal to dislodge or scrap out sample material, as any grooves or scratches in the vessels will increase the risk of contamination.
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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
- Wearing nitrile gloves, wash the individual pieces of the grinding vessels with DI water and a small piece of a scouring pad (no soap).
- After each washed piece piece immediately spray it with isopropyl alcohol and wipe it down with a Kim Wipe. Do not use the ship's compressed air line to dry pieces as the air is too dirty.
- Lay the pieces on, and cover vessels with Kim Wipes.
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 (~3 min should be okay).
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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