User:Karlena L. Brown/Notebook/PVOH Research/2013/02/08

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(PVOH Film Preparations)
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==PVOH Film Preparations==
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==OBJECTIVES==
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'''Prepared PVOH films in water:'''
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* Continue preparing polyvinyl alcohol microspheres for experimental analysis
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* In 10mL beaker, weigh out ~ 0.5 grams PVOH (MW 130,000)
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* Dilute Rhodamine 6G dye solution down to 1μM concentration for prepared microspheres
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'''(Actual Mass = 0.4934g)'''
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* Prepare DSC samples for polyvinyl alcohol microspheres created
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* Then, using a graduated cylinder add ~ 3 mL H<sub>2</sub>O to the beaker
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* In another 10mL beaker, weigh out ~ 1.0 gram PVOH (MW 130,000)
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'''(Actual Mass = 0.9965g)'''
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* Then, using a graduated cylinder add ~ 5 mL H<sub>2</sub>O to the beaker
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'''Standard PVOH Film Protocol:'''
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==Microsphere PVOH 146K 110% CEC Laponite w/ DMHXLBR Information==
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* After adding and combining PVOH (MW 130,000) in small beakers with H<sub>2</sub>O, add stir bars and prepare to stir solution.
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{| {{table}}
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* On hot plate, stir and heat both beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves.
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| align="center" style="background:#f0f0f0;"|'''Preparation of Microspheres using PVA MW 146,000-186,000'''
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* Once PVOH solids thoroughly dissolve in solution, pour each solution in a Teflon dish to sit, cool, and dry in a fume hood for ~ 1 day.  
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Amount of PVA added(g)||0.9001
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|-
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| Amount of Lamponite clay added(g)||0.1004
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|-
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| Amount of cellulose acetate butyrate added(g)||0.6066
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|-
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| Amount of GA added(mL)||0.75
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|-
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| Amount of H2SO4 added(mL)||0.25
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|}
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<br>
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'''Notes:'''
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==Rhodamine 6G Dye Dilution Calculations==
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* An additional 2-3 mL H<sub>2</sub>O was added to each solution to aid the dissolving of the PVOH  
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'''1μM Rhodamine 6G Dye Concentration'''
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* Heat was reduced when solutions began to boil too rapidly
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  M<sub>1</sub>V<sub>1</sub> = M<sub>2</sub>V<sub>2</sub>
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* While transferring solutions to Teflon dishes, loss of sample within the small beakers (sample loss = incomplete sample transfer)
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  1μM (RG6)x 25mL = (92μM)V<sub>2</sub>    V<sub>2</sub> = 271.74μL
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==DSC Analysis: Exchanged Clays & PVOH 146K Microspheres==
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'''DSC preparation and protocal involving instrumentation and usage can be found on 9/17/12 entry.'''
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Sample Name'''
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| align="center" style="background:#f0f0f0;"|'''Sample Mass (mg)'''
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| align="center" style="background:#f0f0f0;"|'''Pan / Lid Mass (mg)'''
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|-
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| NaMT||3.16||48.13
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|-
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| 50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||2.90||48.91
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|-
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| 110% CEC NaMT w/ DMHXLBR||3.01||50.14
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|-
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| Laponite||3.06||50.18
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|-
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| 110% CEC Laponite w/ DMHXLBR||3.08||49.52
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|-
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| 90:10 PVOH 146K Laponite Dust||2.89||48.87
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|-
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| 90:10 PVOH 146K Laponite Medium Clumps||2.96||48.89
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|-
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| 90:10 PVOH 146K Laponite Large Clumps||3.07||48.18
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|}
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==Notes==
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* After preparing the microspheres from the PVOH 146K Laponite, many of the spheres were not spherical. Large clumps of all sizes were produced rather than microspheres.
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* The microspheres prepared from PVOH 146K Laponite were rigid white crystalline structures with stacked layers.
 +
* Due to large sizes of the microspheres, they had to be ground up using a mortar and pestle before adding the 1μM rhodamine 6G dye solution.
 +
* Also DSC was taken of the different sizes of the microspheres to determine if the structure, function, and capability of the microspheres had changed due to extensive clumping.
 +
* When going through the process of preparing new microspheres from PVOH 146K 110% CEC Laponite w/ DMHXLBR, due to slowed vacuum filtration the sample was placed in a vial with the last solvent used for cleaning, methanol.
 +
* When freezing the new microsphere sample in liquid nitrogen, PVOH 146K 110% CEC Laponite w/ DMHXLBR, it was frozen in a medium of methanol and vacuum filtrated to remove the methanol residue.

Revision as of 01:41, 11 February 2013

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OBJECTIVES

  • Continue preparing polyvinyl alcohol microspheres for experimental analysis
  • Dilute Rhodamine 6G dye solution down to 1μM concentration for prepared microspheres
  • Prepare DSC samples for polyvinyl alcohol microspheres created

Microsphere PVOH 146K 110% CEC Laponite w/ DMHXLBR Information

Preparation of Microspheres using PVA MW 146,000-186,000 '
Amount of PVA added(g)0.9001
Amount of Lamponite clay added(g)0.1004
Amount of cellulose acetate butyrate added(g)0.6066
Amount of GA added(mL)0.75
Amount of H2SO4 added(mL)0.25


Rhodamine 6G Dye Dilution Calculations

1μM Rhodamine 6G Dye Concentration

  M1V1 = M2V2
  1μM (RG6)x 25mL = (92μM)V2    V2 = 271.74μL

DSC Analysis: Exchanged Clays & PVOH 146K Microspheres

DSC preparation and protocal involving instrumentation and usage can be found on 9/17/12 entry.

Sample Name Sample Mass (mg) Pan / Lid Mass (mg)
NaMT3.1648.13
50% CEC NaMT w/ Bu3HdP+2.9048.91
110% CEC NaMT w/ DMHXLBR3.0150.14
Laponite3.0650.18
110% CEC Laponite w/ DMHXLBR3.0849.52
90:10 PVOH 146K Laponite Dust2.8948.87
90:10 PVOH 146K Laponite Medium Clumps2.9648.89
90:10 PVOH 146K Laponite Large Clumps3.0748.18

Notes

  • After preparing the microspheres from the PVOH 146K Laponite, many of the spheres were not spherical. Large clumps of all sizes were produced rather than microspheres.
  • The microspheres prepared from PVOH 146K Laponite were rigid white crystalline structures with stacked layers.
  • Due to large sizes of the microspheres, they had to be ground up using a mortar and pestle before adding the 1μM rhodamine 6G dye solution.
  • Also DSC was taken of the different sizes of the microspheres to determine if the structure, function, and capability of the microspheres had changed due to extensive clumping.
  • When going through the process of preparing new microspheres from PVOH 146K 110% CEC Laponite w/ DMHXLBR, due to slowed vacuum filtration the sample was placed in a vial with the last solvent used for cleaning, methanol.
  • When freezing the new microsphere sample in liquid nitrogen, PVOH 146K 110% CEC Laponite w/ DMHXLBR, it was frozen in a medium of methanol and vacuum filtrated to remove the methanol residue.



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