February 10, 2015
1. Stop oxidation reaction that was set up yesterday
2. Analyze the products of the reaction
3. Determine the mass of the nano fibers that were dried out
4. Assist Alicia in setting up her polymerization reaction
5. Prepare more 30:1 Colloid
- The experiment was set up in a 50 mL double-neck pear bottom flask and attached to a reflux condenser the previous day
- Inside the flask there was 3 mL solution prepared from:
- 1 mmol 30% H2O2 (0.333 mL)
- 1 mmol Benzhydrol (0.608 g)
- Dissolved in 10 mL ethanol
- The reaction was stopped by adding water in excess to form the white solid product (Bezophenone)
- The white solid product was filtered and weighed to have a final weight of 0.14336 g.
- The theoretical yield was calculated using:
- C13H12O + H2O2 → C13H10O + 2H2O
- Limiting reagent : 1 mmol 30% H2O2
- 1mmol C13H10O * (182. 217 g/ mol) = 0.182217 g Benzophenone
- The final amount of benzophenone yielded was 78.68%
- The white solid was then dissolved in ethyl acetate and centrifuged to separate the gold nanoparticles from the solution.
- A TLC plate was spotted with the starting material (minus the addition of the colloid) and the final reaction mixture for comparison.
- Further analysis will include column chromatography using hexane and chloroform as an eluent (4:1) and NMR.
- The mass of the AuNPs was determined by Jacob Esenther and the methods can be found in his laboratory notebook
- Alicia set up her polymerization of aniline reaction on the schlenk line.
- More 30:1 Au:Lys colloid was prepared:
- The colloid was prepared as described on January 27,2015
- A total of 20 vials were prepared
A silica gel column will be poured for column chromatography and the samples on the TLC plates will be used for NMR tomorrow.
The 30:1 colloid solutions that were prepared on February 4,2015 formed fibers. The maximum threshold for colloid in solution is 35:1 so we there could have been a pipetting error when we added the lysozyme.