User:James C. Schwabacher/Notebook/Protein-Templated Quantum Dots/2014/10/08

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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 using new sodium sulfide nonahydrate
    1. .048036 g of sodium sulfide nonahydrate (MW=240.18) needed for 10 mL
    2. Used .0488 g of Sodium Sulfide used (in 10 mL) for a 20.32 mM solution
  2. Degassed solution by bubbling N2 gas through for 40 minutes
  3. Add 4 mL of 20 mM sodium sulfide solution to reaction
    1. Allowed the mixtures to stir vigorously for 15 minutes
    2. removed 1 mL aliquot for analysis
    3. Poured contents (minus the stir bar) into a darkened falcon tube and filled with 200 proof ethanol to the 50 mL mark. The falcon tube was left in the freezer to begin precipitation.
    4. total synthesis time JCS 4: 11 hrs (including 15 minutes for Sodium Sulfide addition)


Notes

  • JCS 6 remained a pale yellow that turned dark brown once Na2S was added.