Objectives
- Make 0.8 wt% glutaraldehyde in PVOH (MW 22000) film.
- Exchange 2.0 g Na-MT with 100% tributyl(hexadecyl)phosphonium bromide (Bu3HdP+).
- Exchange 2.0 g Na-MT with 50% (Bu3HdP+).
- Make 2.0 g Na-MT coated with Fe3O4 in a 2:1 ratio of Na-MT to Fe3O4.
- Run DSC on crosslinked and uncrosslinked PVOH (MW 22000) films.
Clay Preparation
General protocol for 100% Bu3HdP+ Sodium montmorillinite(NaMT) exchange:
- In a 50mL Eerlenmeyer flask, weigh out ~ 2 grams of clay(NaMT)
- Add appropriate amount of Bu3HdP+
- Place stir bar in Erlenmyer flask
- Using a graduated cylinder add ~25mL of deionized H2O and ~25mL ethanol to clay and surfactant
- Place flask on a stir plate and close the flask with a rubber stopper
- Allow to stir for ~1 week
Preparation of 100% Bu3HdP+(NaMT) exchange:
2.0095 g Na-MT x (92 meqv/100 g Na-MT) x (1 mol Bu3HdP+/1000 meqv) x (100/100)% x (507.65 g Bu3HdP+/1 mol Bu3HdP+) = 0.9385 g Bu3HdP+
- Actual Bu3HdP+ Mass = 0.9399g
- Actual mass of NaMT used= 2.0095g
General Protocol for 50% Bu3HdP+(NaMT) exchange:
- Repeat steps in general protocol of 100% exchange BUT use only half of the amount of Bu3HdP+
Preparation of 50% Bu3HdP+(NaMT) exchange:
2.0046 g Na-MT x (92 meqv/100 g Na-MT) x (1 mol Bu3HdP+/1000 meqv) x (50/100)% x (507.65 g Bu3HdP+/1 mol Bu3HdP+) = 0.4682 g Bu3HdP+
- Mass of NaMT used= 2.0046g
- Mass of Bu3HdP+ used = 0.4690g)
Fe2O3 coated NaMT preparation
General Protocol:
- In a 50mL Erlenmyer flask, place 2g NaMT and a magnetic stirrer
- In the same 50mL Erlenmyer flask add ~1g FeSO4
- Add ~1g FeCl3
- Add 40mL deionized H2O to Erlenmyer flask
- Add 10mL 5M NaOH to the solution dropwise while stirring the solution
- ~30 minutes after stirring filter the solution
- Using 41 Whatman filter paper, the solution was filtered and the clay was collected
Notes:
- Upon precipitating the Fe, the solution turned a dark brown/ blackish solution
- The Erlenmyer flask was rinsed with deionized H2O
Glutaraldehyde film preparation
General Protocol:
- Follow general protocol for PVOH film preparation described 8/29/2012
- Once all of PVOH solid dissolves, take the beaker and place under the fume hood
- Allow the solution to cool to ~50°C
- Add 0.8wt% glutaraldehyde to the solution
- Allow the solution to stir for ~3 minutes with minimal heat
- Pour the solution into a Teflon dish to sit and cool for ~ 2 days.
- Note: The Teflon dish must remain in the fume hood
Glutaraldehyde safety:
- Glutaraldehyde is highly toxic. Care must be used at all times when dealing with glutaraldehyde
- Avoid all glutaldehyde skin contact by wearing gloves and googles
- Glutaldehyde should be kept in the freezer when not in use
- When in use, glutaldehyde should be kept in the fume hood
- Keep the glutaldehyde vial in a beaker so that it does not spill
- If spilled, wipe up glutaldehyde with paper towel while wearing gloves
- Keep all spills of glutaldehyde contained in the fume hood
- Wash hands after removing gloves that were in contact with glutaldehyde
- Any film with traces of glutaraldehyde must be contained in the fume hood
- Glutaraldehyde is a colorless liquid, but emits a distinctive odor
- Glutaraldehyde is most toxic through inhalation. When in use, try not to breathe as frequently when using the liquid
Preparation:
Actual mass PVOH(MW 22000) used= 0.5141g
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