Objectives
- Crosslink the prepared glutaraldehyde film
- Run DSC on 3 films
- Run FTIR
Crosslinking of Glutaraldehyde film
General Protocol:
- Allow the glutaraldehyde PVOH film to completely air dry
- Prepare a solution of 100mL H2O, 2mL concentrated H2SO4, and 20g Na2SO4 in a 150mL beaker. Place stir bar in beaker and a Buchner funnel top over the stir bar
- Heat the prepared solution to 70°C(on hot plate turn temperature to 160°C)
- Place film in solution for 1 hour.(Make sure the temperature remains at 70°C)
- Prepare 100mL 1% aqueous HCl solution. Heat solution to 70°C
- Remove film from the solution and rinse with deionized H2O
- Place stir bar in 1% HCl solution and a Buchner funnel top over of the stir bar. Add the PVOH film to the solution
- Allow film to remain in 1% HCl solution for 30 minutes.(Be sure to keep a constant 70°C)
- Prepare 0.2M sodium bicarbonate solution
- After 30 minutes, remove film from 1% HCl solution and place in 0.2M sodium bicarbonate solution for ~15minutes
- Remove film from dilute sodium bicarbonate solution with tweezers. Rinse with deionized H2O and dry film on paper towel(dabbing gently).
- Weigh PVOH film. Record mass
Solution Preparations
'
|
Solution 1
|
1% Aqueous HCl
|
0.2M Sodium Bicarbonate
|
Mass Na2SO4 added(g) |
20.0050 |
0 |
0
|
Amount of [H2SO4]added (mL) |
2.00 |
0 |
0
|
Amount of [HCl] added(mL) |
0 |
1.00 |
0
|
Amount of Sodium Bicarbonate(g) |
0 |
0 |
1.6804
|
Note:
- After treatment with solutions, the glutaraldehyde film had a mass of 0.5126g
- After treatment with solutions, the glutaraldehyde film had more of a rubber like texture and was less transparent
DSC on Crosslinked PVOH MW(22,000) films
Films were put in the DSC following the standard protocol
- Crosslinked PVOH (MW 22000):
- Pan mass: 49.14 mg
- Sample mass: 3.07 mg
- Crosslinked PVOH (MW 22000), 10% maleic acid, HCl:
- Pan mass: 50.57 mg
- Sample mass: 3.14 mg
- Crosslinked PVOH (MW 22000), 10% succinic acid, HCl:
- Pan mass: 49.01 mg
- Sample mass: 2.86 mg
FTIR on PVOH(MW 22,000) Thin Film
- Note: It is necessary to redo this analysis. The scan losses resolution around 3700 to 3000 cm-1, indicating that the film is too thick for FTIR. A thinner film of the same MW will be prepared and analyzed
DSC run today
- Using the standard protocol of DSC described on 9/12/2012, the following films were analyzed using DSC:
- PVOH (MW 22000)
- Crosslinked PVOH (MW 22000)
- PVOH (MW 22000), 10% succinic acid, HCl
- PVOH (MW 22000), 10% maleic acid, HCl
- Crosslinked PVOH (MW 22000), 10% maleic acid, HCl
- Crosslinked PVOH (MW 22000), 15% succinic acid, H3PO4
- Crosslinked PVOH (MW 22000), 15% maleic acid, H3PO4
- Crosslinked PVOH (MW 22000), 10% succinic acid, HCl
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