- Complete the QD syntheses begun yesterday
- Attempt precipitation of JCS 4 and 5 via rotovap
- Create 20 mM sodium sulfide solution
- .024018 g of Sodium Sulfide (MW=240.18) needed for 5 mL
- Used .0766 g of Sodium Sulfide used (in 10 mL) because the sample is contaminated with excess water
- Add 4 mL of 20 mM sodium sulfide solution to each reaction
- Allowed the mixtures to stir vigorously for 15 minutes
- total synthesis time JCS 4: 11.5 hrs (including 15 minutes for Sodium Sulfide addition)
- Total synthesis time JCS 5: 11.5 hrs (including 15 minutes for Sodium Sulfide addition)
Precipitation of JCS 4 and 5
- Solutions were transferred to larger, 100 mL round-bottom flasks
- Each solutions was rotovapped for over 30 minutes under vacuum in a water bath of 40 °C
- Resulting films were left in the round bottom flasks, covered with aluminum foil, capped, and stored in a drawer for work-up later in the week.
- JCS 4 remained a very light gray that turned dark brown once Na2S was added.
- JCS 45 remained a strong yellow that turned dark brown once Na2S was added
- JCS 3 remains in an ethanol-water mixture in the freezer