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Each sample will correspond to one beaker; collect as many as needed. Beakers need to be cleaned (DI water and isopropyl alcohol) and labeled ( ex. 1, A, or sample label).
Next start the grinding process using the Buehler grinder located in the Xray prep area of the thin section lab (Figure 1).
Note: The diamond disc is attached to a magnetic disc which is then placed on the wheel plate.
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To start the polisher flip the 'On' switch in the back (Figure 1A). The power indicator light (Figure 1B) should illuminate. Press the timer on/off button (Figure 1C) to get continuous disc rotation. Turn the water on by flipping the 'Water' switch to the 'On' position (Figure 1D). The water flow can be adjusted by turning the knob shown in Figure 1E.
The rotation speed is controlled by the dial shown in Figure 1F. The range is 0 rpm to 500 rpm. 150 rpm is a good starting position. Adjust the speed if needed: faster for hard rocks and slower for softer rocks.
With the water on and the RPM adjusted press the 'Run' button (Figure 1G). Move the sample back and forth across the disc to prevent making a groove. If there is an emergency press the 'Emergency Stop' button (Figure 1H) to stop rotation and cut off the water. To enable the wheel again twist the knob until it pops back out.
Polish the rocks with a Breuler diamond disc (Figure 2) until they're completely smooth and round on all edges. The purpose of grinding on a diamond disc is to remove any possible contaminates caused by the drilling mud (or drill bit) along with the rock saws in the splitting room. There should no pits or jagged corners. Put the rock into a labeled beaker (Figure 3) and polish the next sample. Do this for all samples and then move on to 'Cleaning Samples'.
Figure 2. Buehler diamond discs for polishing (use either one, or start with the courser grain grained and finish with finer grain).
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Pour either DI water or isopropyl alcohol (70%) into the beaker to cover the sample. Check with the scientists for their preference in solution. There should be enough liquid to keep the sample from floating in the sonic bath (Figure 3).
Figure 4. Sonic Bath
Fill the sonic bath (Figure 4) with a little bit of water and place beakers inside. Sonicate for 15 minutes. You should notice the water becoming cloudy from residue being shaken off the samples. Then follow the wash sequence below:
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Repeat the rinse cycle until the water is clear. If the samples are soft and/or clay rich, they won't reach the "clear water" state. Continuing to sonicate will only dissolve the sample. If after 3–4 washings, the water still isn't clear, go to the next step. After the final rinse, decant as much water from the beaker as possible.
Drying Samples
This step involves an overnight portion and requires at least 12 hours and therefore should be done towards the end of the your shift.
Apparatus and Materials
- ICP Prep Oven
- Samples
Place the beakers into the ICP Oven at 110°C for 12 hours (Figure 4). Turn on the power button and adjust the knob to 110°C, which is marked on the oven. A thermostat is located inside to double check temperature.
Turn oven on and adjust the dial to about 110°C. The dial should always be set at that temp. Turn on and confirm the oven temp via the thermostat inside the oven. It is important to not overheat the sample as it may affect some minerals. Less than 110°C is ok, but it may take longer than 12 hours for the sample to dry.
Apparatus and Materials
- ICP Prep Oven
- Samples
Note: The ICP oven should be kept clean at all times, as samples are left open and are susceptible to contamination. The ICP oven should only be used for ICP samples. If the oven shows any sign of rusting, please notify the ALO as a new oven will need to be ordered.
Place the beakers into the ICP Oven at 110°C for at least 12 hours (Figure 5). You can cover the beakers with a larger clean beaker if there is any possibility of rust or debris falling onto the sample.
Figure 5Figure 4. The ICP Prep Oven located in the X-Ray lab. A. ‘On/Off’ Switch B. Temperature Setting C. Heating Indicator.
After 12 hours hours the samples should be dry, remove the beakers from the oven and place them inside the desiccator (Figure 56) while you prepare the X-press station.
Note: The ICP oven should be kept clean at all times, as samples are left open and are susceptible to contamination. The ICP oven should only be used for ICP samples.
Figure 56. Desiccators located in the X-ray lab
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The X-Press is a motorized hydraulic press that crushes samples into smaller pieces.
First, clean the X-press with simple green and isopropyl alcohol. Clean the work area and all materials with isopropyl alcohol for each sample.
Place Place a large KimWipe on your working surfaces for your clean materials. Next collect the following supplies that make up the 'crushing unit' of the X-press (Figure 67). Materials are located in the drawer labeled 'X-PRESS SUPPLIES' in the X-Ray Prep Area in the thin section labThin Section Lab.
- Weigh Weighing Paper 6" x 6"
- Core liner
- Two delrin discs
- Stainless steel base
- Aluminum Die
Figure 67: Materials needed for assembly of ‘crushing unit’. A. Weigh Weighing Paper 6”x6”. B. Core Liner C. Two Delrin Discs D. Stainless Steel Base E. Aluminum Die.
Put on gloves and 'wash' them your gloved hands with isopropyl alcohol. Clean the crushing supplies with isopropyl alcohol and set them down on the clean surface.
Collect Collect sample beakers from the desiccator. Put a piece of parafilm over each beaker and bring them over to the X-press.
Now Now that the X-press area is clean and the samples are in the lab, assemble the crushing unit as follows:
- Grab the stainless steel dish. This is the base for the crushing unit (Figure 78).
Figure 78. Stainless steel dish
- Place a piece of Weigh Paper on the Base (Figure 89).
Figure 89. Dish with Weigh paper
- Put one Delrin disc on top of the weigh paper (Figure 910).
Figure 910. Delrin Disk disk Added
- Place the sample on top of the Delrin Disc (Figure 1011). These discs can fracture leaving Teflon flakes in the sample so arrange the sample such that the two flattest surfaces are the top and bottom.
Figure 1011. Sample Added
- Now place the second delrin disc on top of the sample (Figure 1112). Again make sure the disc rests flat against sample.
Figure 1112. Second Delrin Disk added
- Put the aluminum die on top of the delrin disk, holding it until you slip the core liner over the unit (Figure 1213).
Figure 1213. Aluminum Die added
- Now slip the piece of core liner over all the pieces and resting inside the stainless steel base (Figure 1314). This contains the sample pieces inside the unit.
Figure 1314. Core Liner added
- The crushing unit is now assembled and we can start crushing samples (Figure 1415).
Figure 1415: Overview of the X-Press. A. Metal platform sample rests on B. Jacksrew C. Pressure Relief Handle. D. ‘On’ toggle E. Pressure Gauge.
Place the crushing unit inside the X-Press in the middle of the metal platform (Figure 14 A15A). Put in the sliding polycarbonate door down when crushing samples. Tighten the jackscrew (Figure 14 B15B) until it rests firmly against the aluminum die. Tighten the 'pressure relief handle' with a clockwise turn (Figure 14 C14C).
Note: The polycarbonate door sits on two interlock switches that enable operation. If the door is not fully closed or pressing down on these switches the machine will not work.
Crush the sample by continuously holding down the toggle switch (Figure 14 D14D). The motor and pump can be heard and the pressure will rise (Figure 14 E14E). Once the desired pressure is reached the toggle can be released and the sample will sit under that pressure. Do NOT leave a sample under pressure for any reason. For most samples ~5 tons of pressure is enough force to crack it. If you find the need to go near 10 tons, try rotating the sample onto another side and repeat the process again. Taking the pressure up greater than 10 tons can cause the disks and the core liner to shatter. Contaminating the samples and creating a safety hazard.
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After the sample has cracked remove the crushing unit. To remove the unit, loosen the 'pressure relief handle' (Figure 15C) by rotating it counter clock wise and press 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 and start unscrewing the jackscrew. Then open the door 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.
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Turn on the Shatterbox by flipping the 'On' switch located on the back panel (Figure 15A16A). The control panel is located on the front of the lid next to the handle (Figure 15C).
Figure 1516. Shatterbox. A. Power switch. B. Cover. C. 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 mLs of material and has three components: container, puck and lid (Figure 1617).
Figure 1617. Small vessel components. A. Container B. Puck. C. Lid.
The large grinding vessel holds between 20 – 60mLs of material and has five components: a container, puck, inner ring, O-Ring and lid (Figure 1718).
Figure 1719. Large Vessel components. A. Container B. Inner Ring C. Puck D. O-Ring E. Lid.
The small vessels have a small indent in the bottom of the container and they will sit in the shatterbox resting on either a three-pinned plate (Figure 1819) or a one-pinned plate (Figure 1920).
Figure 1819. Three-pinned rack plate to hold three small vessels in Shatterbox
Figure 1920. Single-pinned rack plate to hold one small vessel in Shatterbox
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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 2021). There can't be any material on top of the puck or inside the sealing ring; 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.
Figure 2021. Small vessel filled with sample pieces. No sample material is on the top the puck or in the lid ring.
Open the lid, pull out the lever arm (Figure 21A22A), and pull up the clamp arm (Figure 21B22B). This will reveal full access to the inner capsule (Figure 21C22C).
Figure 2122. The inside of the Shatterbox. A. The lever arm B. The clamp arm C. The inner capsule 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 (Figure 2223). For crushing two samples, two vessels will be full, whereas the third will be empty without a puck or you can add quartz sand to the third container. It is important to maintain balance within the machine to prevent damage.
Figure 2223. Inside the Shatterbox with the bottom three-pinned rack plate resting inside the inner capsule.
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Now load vessels onto the plate (Figure 2324). The divet in the bottom of the vessels will settle onto the pins and fit firmly in place.
Figure 2324. Three samples loaded into the Shatterbox.
Put the top rack plate over the vessels. Bring down the clamp arm (Figure 24A25A). The guide on the clamp arm will settle into the boss (Figure 24B25B) when centered properly.
Figure 2425. The top rack plate sitting on top of the three samples. A. Clamp arm. B. the “boss” of the rack plate, where the clamp arm will attach.
Bring the lever arm down and push it into the end of the clamp arm (Figure 25B26B). Then push the lever arm down over the clamp arm (Figure 25A26A).
Figure 2526. 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 (Figure 26A27A). Rotating the guide clockwise decreases resistance; whereas counterclockwise increases resistance.
Figure 2627. The lever arm and the guide. A. Retractable locking pin being pushed to allow adjustment of the 'guide' length.
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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 (Figure 27A28A). Adjust the time by pressing on the 'Minute' (Figure 27B28B) and 'Second' (Figure 27C28C) buttons. The timer maximum is 9:59.
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