User:Eleni N. Kalivas/Notebook/CHEM-571/2014/04/08

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Objective

  1. UV-vis and fluorescence of all 6 QD synthesis from 04/02/14.
  2. Make BSA solution 0.1459mM
  3. De-gas all solutions
  4. Synthesis using Gonzalez Method
  5. Continue precipitation of 78% BSA by mass (second trial)
  • BSA made using 0.2409g in 25mL --> 0.1459mM BSA

Protocol

This protocol was taken from Matt Harting's notebook, all solutions de-gassed before synthesis.

  1. To a 3-necked flask is added
    1. 25mL of 20 mM L-cysteine (roughly 22% L-Cysteine)
    2. 25mL .1459 mM BSA (roughly 78% by mass)
    3. 5mL of 100mM ZnSO4 (0.5 mmol)
    4. 5.437mL of 10.3mM MnCl2 (0.056 mmol)
    5. The pH of this mixture is adjusted to 11 with ~1M NaOH (should be on the order of 60uL)
  2. This mixture is stirred under Ar (I'll use N2) for 30 minutes
  3. 5.505mL of 101mM Na2S is quickly added.
  4. The solution is stirred for 20 minutes
  5. The solution is then aged at 50C under air for 2 hours.

Stock Solution Prep

The solutions created for 78%BSA by mass with L-Cysteine synthesis:

  1. 250mL of 20mM L-cysteine
    1. FW 121.16g/mol
    2. measure out: 0.6058g
    3. measured: 0.6072g
    4. actual conc: 20.05mM
  2. 50mL of 100mM ZnSO4
    1. FW 287.56g/mol
    2. measure out: 1.4378g
    3. measured: 1.4399 g
    4. actual conc: 100.1 mM
  3. 50mL of 10mM MnCl2
    1. FW 197.9g/mol
    2. measure out: 0.09895g
    3. measured: 0.0987g
    4. actual conc: 9.98 mM
  4. 10mL 1M NaOH
    1. FW 40.00g/mol
    2. 0.4284g
    3. Final concentration a bit over 1M check pH carefully when adjusting!
  5. 25mL 100mM Na2S
    1. FW 240.18g/mol
    2. measure out: 0.600g
    3. measured: 0.610g
    4. actual conc: 101.6 mM
  6. 25mL .1484 mM BSA





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