User:James C. Schwabacher/Notebook/CHEM-571/2014/02/05

Biomaterials Design Lab

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Protocol Synthesize new nano crystals following the protocol used on Jan 01, 2104 Synthesize new nano crystals using new ligand GSH Attempt new synthesis method described below Preparation of 10uM GSH 0.00278 g in 50mL --> Stock 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 To a 3-necked flask is added 50mL of 20mM L-cysteine 5mL of 100mM ZnSO4 (0.5 mmol) 5.437mL of 10.3mM MnCl2 (0.056 mmol) The pH of this mixture is adjusted to 11 with ~1M NaOH (should be on the order of 60uL) This mixture is stirred under Ar (I'll use N2) for 30 minutes 5.505mL of 101mM Na2S is quickly added. The solution is stirred for 20 minutes The solution is then aged at 50C under air for 2 hours. Results 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.