Objective
- Testing Sol-gel formation of JCS 15 and JCS 16
- Filtering and prepping samples (JCS 15, 16) for characterization
Protocol
- A few mL of millipore water were added to the dried round bottoms
- The round bottoms were swirled gently as more water was added until structures formed.
- Mass of dry JCS 16 round bottom= 67.873g, Mass of dry film is thus .0999g
Observations
- JCS 15, the sample that lacked BSA, formed black precipitate, as expected. There was a minimal amount-- not enough for characterization with pXRD.
- JCS 16, the sample that was not mixed over-night (for a synthesis time of approximately 15 minutes), produced the film-like structures that were discovered serendipitously last semester.
- The resulting structures were separated using filtration with a membrane: Supor-450 47mm 0.45μm
- a 10 mg sample was prepared for DSC analysis (mass of lid+pan: 49 mg, mass of lip+pan+sample: 59 mg)
- The mass of the filter (before filtration) was 0.0671g
- The mass of the filter and sample (after filtration) was 1.411g
- The sample yield was approximately 1.3439g
- Estimated mass of water withheld in structures 1.3439-.0999g= 1.244g
Next Steps
- Conduct a series of 15-min syntheses reducing concentrations of mercury and sulfide by a factor of 10.
- Perform DSC and pXRD on Samples
- Attempt to get BSA-only and BSA-Hg only samples control studies.
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