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- Sonicator with basket
- Beakers
- 70% Isopropyl Alcohol
- Tray(s)
Pour either DI water or Place the basket in the sonic bath and fill to just above the wholes in the basket with DI water. Pour enough isopropyl alcohol (70%) into the each beaker to cover the sample. Check with the scientists for their preference of solutionDI water can also be used if the scientists prefer. Place the beakers in the sonic bath basket. There should be enough liquid in the beaker to keep the sample from floating in the sonic bath basket (Sonic Bath without basket Figure 4).
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Figure 4. Sonic Bath (without basket).
Fill the sonic bath with water and place beakers inside. Sonicate Sonicate the samples for 15 minutes. You should notice the isopropyl or water becoming cloudy from residue being shaken off the samples. Then follow the wash sequence below:
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Open the Excel File LOI_Spreadsheet in Local Disk > DATA >LOI > Documents > XRD > Sample and ICP Prep > LOI > LOI Spreadsheets > LOI_SpreadsheetExpXXX.xlsx
The spreadsheet has three sheets:
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- The second sheet is for repeats.
- The third sheet is the format for uploading the data using the spreadsheet uploader (Figure 41).
Put your LOI information into the spreadsheet following the example format. Fill in the following:
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- Wash the crucibles with DI water and a small piece of a scouring pad (no soap).
- Rinse several times with DI water.
- Place crucibles in a 10% HNO3 bath for 12 hr. If in urgent need, the quartz crucibles can be soaked a minimum of 2 hours, but extra flux blanks will need to be made and added to batches that use these crucibles.
- Rinse the quartz crucibles 3 times with DI water after the acid bath. For the ceramic crucibles, rinse 3 times with DI and then soak them in a large beaker of DI water for 4-6 hours.
- Dry the quartz either type of crucibles in the oven at a maximum temperature of 60°C. Heat For the alumina ceramic crucibles, heat them to 800°C in the muffle furnace for 2 hours and allow to cool to room temperature before removing.
Some crucibles will develop a thin white or red cloudy film, become spotted, or start flaking. If any of these things happen discard the crucible in the sharps container. When the crucible undergoes one of those changes the quartz has started to react at high temperatures, and could start contaminating the samples.
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