User:Moira M. Esson/Notebook/CHEM-581/2012/09/14

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Objectives

  • Crosslink the prepared glutaraldehyde film
  • Run DSC on 3 films
  • Run FTIR

Crosslinking of Glutaraldehyde film

General Protocol:

  1. Allow the glutaraldehyde PVOH film to completely air dry
  2. 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
  3. Heat the prepared solution to 70°C(on hot plate turn temperature to 160°C)
  4. Place film in solution for 1 hour.(Make sure the temperature remains at 70°C)
  5. Prepare 100mL 1% aqueous HCl solution. Heat solution to 70°C
  6. Remove film from the solution and rinse with deionized H2O
  7. Place stir bar in 1% HCl solution and a Buchner funnel top over of the stir bar. Add the PVOH film to the solution
  8. Allow film to remain in 1% HCl solution for 30 minutes.(Be sure to keep a constant 70°C)
  9. Prepare 0.2M sodium bicarbonate solution
  10. After 30 minutes, remove film from 1% HCl solution and place in 0.2M sodium bicarbonate solution for ~15minutes
  11. Remove film from dilute sodium bicarbonate solution with tweezers. Rinse with deionized H2O and dry film on paper towel(dabbing gently).
  12. Weigh PVOH film. Record mass


Solution Preparations

' Solution 1 1% Aqueous HCl 0.2M Sodium Bicarbonate
Mass Na2<sub/>SO4<sub/> added(g)20.005000
Amount of [H2<sub/>SO4<sub/>]added (mL)2.0000
Amount of [HCl] added(mL)01.000
Amount of Sodium Bicarbonate(g)001.6804


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

General Observations:

  • The crosslinked PVOH MW22,000+[HCl]+10% maleic acid and PVOH MW 22,000+[HCl}+10% succinic acid after crosslinking turned very rigid, shiny and black

FTIR on PVOH(MW 22,000) Thin Film

Image:FTIR PVOH(22K).JPG

  • 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:
  1. PVOH (MW 22000)
  2. Crosslinked PVOH (MW 22000)
  3. PVOH (MW 22000), 10% succinic acid, HCl
  4. PVOH (MW 22000), 10% maleic acid, HCl
  5. Crosslinked PVOH (MW 22000), 10% maleic acid, HCl
  6. Crosslinked PVOH (MW 22000), 15% succinic acid, H3PO4
  7. Crosslinked PVOH (MW 22000), 15% maleic acid, H3PO4
  8. Crosslinked PVOH (MW 22000), 10% succinic acid, HCl



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