Table of Contents

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Rock samples are prepared for ICP analysis using the following procedures on each sample:

1. Cut to size (see Cutting Samples to Size below)
2. Polish (see Polishing Samples on Diamond Wheel below)
3. Clean (see Cleaning Samples below)
4. Dry (see Drying Samples below)
5. Crush (see Crushing Samples in the X-Press in XRD Sample Preparation Hard Rock )
6. Grind (see Grinding Samples in the Shatterbox in XRD Sample Preparation Hard Rock)

Cutting Samples to Size

To cut samples for the X-Press, use the splitting room rock saws (located in the Core Deck) following these guidelines:

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Note: The diamond disc is attached to a magnetic disc which is then placed on the wheel plate. Diamond disks are located on the stud shelf in the X-Ray ICP preparation area of the Thin Section Lab. Use the silver or purple diamond disc.

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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 Buehler 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) or the rock saws in the splitting room. There should be no pits or jagged corners. Put the rock into a labeled beaker (Figure 3). Before polishing the next sample, clean the diamond disc with a dressing stone. Dressing stones are found in the Splitting Room of the Core Lab. Do this for all samples and then move on to 'Cleaning Samples'.

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Post-ignition measurements should be taken soon (within an hour) after removing crucibles from the furnace. Failure to do so will disrupt the LOI values. Reweigh the crucible plus the ignited sample to determine how much weight was gained or lost. Follow the same weighing procedure as in Pre-ignition Weighing.

1. Record the final weight in the excel spreadsheet under 'CRUCIBLE + IGN SAMPLE WT'. The spreadsheet will populate the columns 'Post Ignition Loss' and '%LOI'.
2. The formula used to calculate LOI is:

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Copy and paste your spreadsheet into that uploader. Click the 'Edit' button and 'Validate Sheet'. This checks and highlights any errors that need to be fixed. When the spreadsheet comes up clean, click 'Lims' and 'Upload'. The sheet will turn green when the measurements are successfully uploaded. The data is now in LIMS under Chemistry > ICP-AES Solids >Expanded LOI.

Cleaning the Quartz Crucibles

1. Wash the crucibles with DI water and a small piece of a scouring pad (no soap).
2. Rinse several times with DI water.
3. Place crucibles in a 10% HNO₃ bath for 12 hr.
4. Rinse 3 times with DI water after the acid bath.
5. Dry the crucibles in the oven at a maximum temperature of 60°C.

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Figure 43. Fused glass bead. 

• An analytical procedural blank of Flux is prepared identically to the samples. The 0.4 g of flux (the pre-weighed flux) is fused with 10µL 0.172 mM of LiBr and dissolved. An additional 0.1 g of flux is NOT added to mimic the TDS of the 0.5 g mix of sample + flux because this would provide an inaccurate quantitation of the impurities introduced by the amount of flux used in preparation of the unknowns.

Weighing the Sample

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Making beads - protocol used during Exp 391

The process described above was not appropriate to make beads during Exp 391. Some samples had recrystallized parts during cooling. We therefore changed the protocol by doubling the flux quantity (i.e., 400 mg of flux was used) and increasing the sample mass to 125 mg (instead of 100 mg). The temperature of the beadmaker was also "increased" to 1220ºC (see /wiki/spaces/LN/pages/7338176106 regarding the beadmaker temperature issue).

Weighing the Sample

Note: This process is typically done by the chemistry technicians.
Weighing the 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.

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Using the Bead Maker during transit is not advised, due to power fluctuation which could cause damage to the Bead Maker electronics.

Making beads - protocol used during Exp 391

The process described above was not appropriate to make beads during Exp 391. Some samples had recrystallized parts during cooling. We therefore changed the protocol by doubling the flux quantity (i.e., 400 mg of flux was used) and increasing the sample mass to 125 mg (instead of 100 mg). The temperature of the beadmaker was also "increased" to 1220ºC (see /wiki/spaces/LN/pages/7338176106 regarding the beadmaker temperature issue).

Cleaning Platinum Crucibles

1. Rinse crucibles with DI water.
2. If beads are stuck to the bottom, sonicate with DI water for 30 min or more.
3. Place crucibles in HNO3 10% bath for 12 hr. If you notice any signs of residue, leave in the acid bath for longer.
4. Clean a Tupperware container with isopropyl alcohol. Lay down sheets of paper towel and large kimwipes.
5. Take crucibles out of the acid bath and rinse with DI water 3 times. Place crucible in the container. If the crucibles require polishing, see Polishing the Platinum Crucibles.
6. Cover all crucibles with a large Kimwipe and place in the drying oven in the Chemistry Laboratory. Leave overnight.
7. When dry remove crucibles and bring into the XRD laboratory. Wrap each crucible in a small Kimwipe and and place back in the safe. Lock the safe after all crucibles have been put back.

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