User:Melissa Novy/Notebook/CHEM-581/2012/09/07

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Objectives

  • Crosslink PVOH films.
  • Make more PVOH (MW 130000) films with strong acid and maleic or succinic acid.
  • Run solubility tests on crosslinked and uncrosslinked PVOH films.
  • Run FTIR and DSC on PVOH films.

PVOH (MW 22,000) Films

' No acid HCl H3PO4
No acid1.01150.51811.0054
10 wt% maleic acid0.5181
15 wt% maleic acid1.0054
10 wt% succinic acid0.5163
15 wt% succinic acid1.0125

PVOH (MW 130,000 Films

' No acid HCl H3PO4
No acid0.99641.0855
10 wt% maleic acid1.0106 (mass of maleic acid: 0.1071)
15 wt% maleic acid1.0373 (mass of maleic acid: 0.1556)
10 wt% succinic acid1.0215 (mass of succinic acid: 0.1021)
15 wt% succinic acid1.0178 (mass of succinic acid: 0.1528)

Solubility of PVOH Films

  • 0.1023 g of uncrosslinked PVOH (MW 22000), 15 wt% maleic acid, H3PO4 was dissolved in 75 mL H2O.
  • The viscosity of the solution was tested:
Trial Time [s]
1246.67
2253.48
3250.68
  • Average time: 250.28 s

DSC on PVOH Films

  • About 3 mg ± 20% PVOH film was placed in a DSC pan.
  • Uncrosslinked PVOH (MW 22000) + 15% maleic acid + H3PO4
    • Pan mass: 49.42 mg
    • Sample mass: 3.13 mg
  • Uncrosslinked PVOH (MW 22000) + 15% succinic acid + H3PO4
    • Pan mass: 51.02 g
    • Sample mass: 3.15 g



  • Procedure:
    1. Equilibrate at 20.00°C.
    2. Ramp 20.00°C/min to 240.00°C.
    3. Ramp 20.00°C/min to 20.00°C.
    4. Repeat steps 2 and 3 one time.

Notes

  • Films were crosslinked in the oven at 120°C for 90 minutes.
  • Crosslinked PVOH films became more rigid and changed color from transparent to faintly yellow-brown.
  • The viscometer used for previous tests was discovered to be cracked. A new viscometer was subsequently used.



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