User:Moira M. Esson/Notebook/CHEM-581/2012/09/12

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  1. Make 0.8 wt% glutaraldehyde in PVOH (MW 22000) film.
  2. Exchange 2.0 g Na-MT with 100% tributyl(hexadecyl)phosphonium bromide (Bu3HdP+).
  3. Exchange 2.0 g Na-MT with 50% (Bu3HdP+).
  4. Make 2.0 g Na-MT coated with Fe3O4 in a 2:1 ratio of Na-MT to Fe3O4.
  5. 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:

  1. In a 50mL Erlenmyer flask, place 2g NaMT and a magnetic stirrer
  2. In the same 50mL Erlenmyer flask add ~1g FeSO4
  3. Add ~1g FeCl3
  4. Add 40mL deionized H2O to Erlenmyer flask
  5. Add 10mL 5M NaOH to the solution dropwise while stirring the solution
  6. ~30 minutes after stirring filter the solution
  7. Using 41 Whatman filter paper, the solution was filtered and the clay was collected


  • 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:

  1. Glutaraldehyde is highly toxic. Care must be used at all times when dealing with glutaraldehyde
  2. Avoid all glutaldehyde skin contact by wearing gloves and googles
  3. Glutaldehyde should be kept in the freezer when not in use
  4. When in use, glutaldehyde should be kept in the fume hood
  5. Keep the glutaldehyde vial in a beaker so that it does not spill
  6. If spilled, wipe up glutaldehyde with paper towel while wearing gloves
  7. Keep all spills of glutaldehyde contained in the fume hood
  8. Wash hands after removing gloves that were in contact with glutaldehyde
  9. Any film with traces of glutaraldehyde must be contained in the fume hood
  10. Glutaraldehyde is a colorless liquid, but emits a distinctive odor
  11. 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