User:James C. Schwabacher/Notebook/Protein-Templated Quantum Dots/2014/10/01

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Objective

  • Complete the QD syntheses begun yesterday
  • Attempt precipitation of JCS 4 and 5 via rotovap

Protocol

  1. Create 20 mM sodium sulfide solution
    1. .024018 g of Sodium Sulfide (MW=240.18) needed for 5 mL
    2. Used .0766 g of Sodium Sulfide used (in 10 mL) because the sample is contaminated with excess water
  2. Add 4 mL of 20 mM sodium sulfide solution to each reaction
    1. Allowed the mixtures to stir vigorously for 15 minutes
    2. total synthesis time JCS 4: 11.5 hrs (including 15 minutes for Sodium Sulfide addition)
    3. Total synthesis time JCS 5: 11.5 hrs (including 15 minutes for Sodium Sulfide addition)

Precipitation of JCS 4 and 5

  1. Solutions were transferred to larger, 100 mL round-bottom flasks
  2. Each solutions was rotovapped for over 30 minutes under vacuum in a water bath of 40 °C
  3. 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.

Notes

  • 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