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

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==Objectives==
==Objectives==
*Crosslink the prepared glutaraldehyde film
*Crosslink the prepared glutaraldehyde film
*Run DSC on 8 films
*Run DSC on 3 films
*Run FTIR
*Run FTIR
==Crosslinking of Glutaraldehyde film==
==Crosslinking of Glutaraldehyde film==
General Protocol:
General Protocol:
#Allow the glutaraldehyde PVOH film to completely air dry
#Allow the glutaraldehyde PVOH film to completely air dry
#Prepare a solution of 100mL water, 2mL concentrated H<sub>2<sub/>SO<sub>4<sub/>, and 20g Na<sub>2<sub/>SO<sub>4<sub/> in a 150mL beaker. Place stir bar in beaker and a buchner funnel top over the  
#Prepare a solution of 100mL H<sub>2</sub>O, 2mL concentrated H<sub>2</sub>SO<sub>4</sub>, and 20g Na<sub>2</sub>SO<sub>4</sub> 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 H<sub>2</sub>O
#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 H<sub>2</sub>O and dry film on paper towel(dabbing gently).
#Weigh PVOH film. Record mass
<br>
'''Solution Preparations'''
{| {{table}}
| align="center" style="background:#f0f0f0;"|''''''
| align="center" style="background:#f0f0f0;"|'''Solution 1'''
| align="center" style="background:#f0f0f0;"|'''1% Aqueous HCl'''
| align="center" style="background:#f0f0f0;"|'''0.2M Sodium Bicarbonate'''
|-
| Mass Na<sub>2<sub/>SO<sub>4<sub/> added(g)||20.0050||0||0
|-
| Amount of [H<sub>2<sub/>SO<sub>4<sub/>]added (mL)||2.00||0||0
|-
| Amount of [HCl] added(mL)||0||1.00||0
|-
| Amount of Sodium Bicarbonate(g)||0||0||1.6804
|}
<br>
'''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<sup>-1</sup>, 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, H<sub>3</sub>PO<sub>4</sub>
# Crosslinked PVOH (MW 22000), 15% maleic acid, H<sub>3</sub>PO<sub>4</sub>
# Crosslinked PVOH (MW 22000), 10% succinic acid, HCl
 
 




Revision as of 21:08, 14 October 2012

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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 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

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

  • 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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