User:Andrew K Farag/Notebook/CHEM-571/2014/02/05

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Objective

  1. Synthesize new nano crystals following the protocol used on Jan 01, 2104
  2. Synthesize new nano crystals using new ligand GSH
  3. Attempt new synthesis method described below


Prepare 10 uM of GSH

  1. 0.00278 g in 50mL --> Stock
  2. 569.13uL Stock in 10mL --> 10 uM GSH


Preparation of BSA-GSH nanocrystal solutions

% BSA 5 mM Zinc Nitrate (uL) 5mM Manganese Acetate (uL) 41.65 mM Ammonium Acetate (uL) 10uM BSA* (uL) 10uM GSH (uL) 10mM Ammonium Hydroxide (uL) 5 mM Sodium Sulfide* (uL) Total Volume (mL)
0 540 60 600 0 600 3000 600 5.4
10 540 60 600 60 540 3000 600 5.4
20 540 60 600 120 480 3000 600 5.4
30 540 60 600 180 420 3000 600 5.4
40 540 60 600 240 360 3000 600 5.4
50 540 60 600 300 300 3000 600 5.4
60 540 60 600 360 240 3000 600 5.4
70 540 60 600 420 180 3000 600 5.4
80 540 60 600 480 120 3000 600 5.4
90 540 60 600 540 60 3000 600 5.4
100 540 60 600 600 0 3000 600 5.4

Protocol for New synthesis method

This protocol was taken from Matt Harting's notebook

  1. To a 3-necked flask is added
    1. 25mL of 20mM L-cysteine
    2. 25mL of 20mM BSA
    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 Na<usb>2</sub>S is quickly added.
  4. The solution is stirred for 20 minutes
  5. The solution is then aged at 50C under air for 2 hours.

Notes

  • 2.53 mL of 1M NaOH, in the future 2mL will be added to adjust the pH.
  • When first adding NaOH it resulted in a cloudy white precipitate, that increased in cloudiness as more NaOH was added, after the last mL was added the solution changed to a clear gold solution.


UV-Vis Results with the new synthesis method
BSA-CYS.png
UV-Vis of BSA-GSH
02.12.UV-Vis.BSA-GSH.png