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Appendix C: Open Vessel Reactions
Perform a Reaction
WARNING
Proper precautions must be taken to avoid contact with solvents or solvent vapors. Protective gear should
be worn as outlined in the user’s safety program for hazardous materials and the solvent manufacturer’s
safety data sheet. Refer to these guidelines for proper handling and disposal of the solvents.
Prepare the Flask
1. Inspect the round bottom ask for any cracks or scratches. Vessels with cracks or scratches need to be dis-
carded and replaced because the structural integrity of the vessel can be compromised.
2. Add the reagents to the ask.
2.1. Place Teon coated magnetic stir bar into the ask.
2.1. Weigh and add the solids.
2.2. Add the solvent. Use the solvent to rinse the inside of the ask to ensure that the sample is in the
base. Do not exceed a volume of 70% of the round bottom ask.
2.3. Ensure that the solvent covers the sample and the base of the ask. A minimum volume of 100 mL
and a maximum volume of 70% of the round bottom ask is required.
3. Verify the oor mat positioning.
4. Place the Teon stand over the turntable drive lug, in the center of the cavity. The support riser is required for
250 mL - 1000 mL round bottom asks to prevent the ask from touching the turntable drive lug.
5. Place the round bottom ask with the reaction on to the vessel stand in the cavity.
6. If applicable, attach extension glassware and a condenser.
7. View the “Fiber Optic Temperature Control” section for detailed instructions on connecting the ber optic probe
and entering the GF number.
8. Insert the ber optic probe through the open I/O port on top of the microwave cavity and into the bottom of the
ask. A thermowell may be used to protect the temperature probe from becoming damaged during the reac-
tion. Contact CEM Corporation for information.
• If the adapter with the temperature probe port is being used, insert the probe through the I/O port.
• If the reux condenser without the temperature probe port is being used, feed the probe through the top of
the condenser down in to the round bottom.
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