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After 12 hours the samples should be dry, remove the beakers from the oven and place them inside the desiccator (Figure 6) while you prepare the X-press station.
Figure 6. Desiccators located in the X-ray lab
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Clean the balance area including the balance plates inside the balance. Any dust or particles on the plate could throw off the weight measurements. Before beginning make sure there are enough acid washed quartz crucibles for your samples. The crucibles are located in the X-Ray lab in a plastic container labeled 'Acid Washed Crucibles'. Wear gloves while handling the crucibles.
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Place a large sheet of paper in front of the balances and place supplies here. For each sample you need weigh paper (Figure 28A), a scoopula (Figure 28C), and a quartz crucible set (Figure 28B). Clean the scoopula with isopropyl alcohol in between each sample as it has direct contact with the sample powder.
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Figure 28. Materials needed for weighing LOI. A: Clean paper or kim wipe. B: Crucible set. C: Scoopula. D: Samples
Setting up the Mettler Toledo Balances
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Figure 29. Mettler Balance Station located in the XRay lab. A: Reference balance. B: Unknown balance. C: Sliding door. D: Reference power module. E: Unknown power module.
Open Open the Mettler Balances program (Figure 30). There are multiple panes and parameters that are set before we start measuring.
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Figure 36. Weighing an empty inner crucible.
Close the door and click 'Weigh'. Wait for the counts to finish and then record the 'Final Weight' in the spreadsheet under 'Crucible Wt'.
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Figure 37. Crucible with approximately 5g of sample. Pre-ignition measurement
When the sample is close to this range click 'Weigh.' Press 'Halt' to stop the measurement and either add or remove sample if needed, and then click on 'Weigh' again to take a new measurement.
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Figure 38. Complete crucible unit with sample, ready for ignition.
Igniting Samples
Samples are ignited in the Thermolyne Muffle furnace located in the Chemistry Laboratory. The entire ignition cycle takes approximately 20 hours to complete and cool down to ~200°C. After ignition, samples need to be taken out when they come down to ~ 50°C-200°C. If the samples sit for too long they will reabsorb moisture and the 'Post-Ignition Weight' will be inaccurate. Time this accordingly.
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Figure 39. The Thermolyne Muffle Furnace. A: Power Switch. B: Control Panel. C: Door handle.
Confirm with scientists, what temperature and how long samples should be run for. Below is a quick reference guide:
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Collect platinum crucibles, platinum tipped tongs, 0.172 LiBr, and pipette tips from the safe above the Bead Maker (Figure 44). 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 44. Bead making supplies. A: Platinum tipped tongs. B: Platinum crucibles. C: 0.172 Libr wetting agent. D: Pipette. E: Teflon spatula. F: Pipette tips.
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Next, turn on the water (Figure 46; 47). The handle is to the left of the machine on the wall. Raise the handle slightly to turn it on. You will hear a small click once it is in the 'on' position. Now the 'Water' and 'Ready' indicator lights should be on. Do not run any samples unless these lights are on.
Figure 46. Water in off position.
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