User:Karlena L. Brown/Notebook/PVOH Research/2013/04/10: Difference between revisions

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==PVOH Film Preparations==
==OBJECTIVES==
'''Prepared PVOH films in water:'''
* Continue fluorescence detection through pressure testing analysis of microsphere samples (new modifications & better results)
* In 10mL beaker, weigh out ~ 0.5 grams PVOH (MW 130,000)
* Continue to run DSC sample analysis on microsphere samples previously prepared on 3/29/13
'''(Actual Mass = 0.4934g)'''
* Continue washing with hexanes and drying microspheres prepared on 03/29/13
* Then, using a graduated cylinder add ~ 3 mL H<sub>2</sub>O to the beaker
* Continue making films containing both clay and PVOH variations to run X-ray analysis
* In another 10mL beaker, weigh out ~ 1.0 gram PVOH (MW 130,000)
'''(Actual Mass = 0.9965g)'''
* Then, using a graduated cylinder add ~ 5 mL H<sub>2</sub>O to the beaker


'''Standard PVOH Film Protocol:'''
==DSC Analysis: Mixed Microspheres 2==
* 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.
'''DSC preparation and protocol involving instrumentation and usage can be found on 9/17/12 entry.'''
* On hot plate, stir and heat both beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves.
* 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.  


'''Notes:'''
{| {{table}}
* An additional 2-3 mL H<sub>2</sub>O was added to each solution to aid the dissolving of the PVOH
| align="center" style="background:#f0f0f0;"|'''Sample Name'''
* Heat was reduced when solutions began to boil too rapidly
| align="center" style="background:#f0f0f0;"|'''Sample Mass (mg)'''
* While transferring solutions to Teflon dishes, loss of sample within the small beakers (sample loss = incomplete sample transfer)
| align="center" style="background:#f0f0f0;"|'''Pan / Lid Mass (mg)'''
|-
| PVOH 130K||3.01||50.15
|-
| PVOH 146K||3.14||49.98
|-
| 50:50 PVOH 130K NaMT||3.03||49.87
|-
| 50:50 PVOH 130K Laponite||2.86||49.94
|-
| 90:10 PVOH 130K 50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||2.89||50.30
|-
| 50:50 PVOH 130K 110% CEC NaMT w/ DMHXLBR||3.13||50.55
|-
| 50:50 PVOH 130K 110% CEC Laponite w/ DMHXLBR||3.17||49.64
|-
| 90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR||2.89||49.48
|-
| 50:50 PVOH 130K 50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||3.04||49.95
|}


* Specific DSC parameters and protocols set to analyze dry clay samples included the following:
    # Equilibrate sample at ~ -40°C
    # Ramp sample temperature up from 20-240°C
    # Ramp sample temperature down from 20-(-40°C)
    # Repeat segment #2 again
==Bent Pipette: Microsphere Pressure Samples Tested==
'''RECALL HYDROGEL PRESSURE TESTING PROTOCOL ON 2/20/13 & FLUORESCENCE ANALYSIS PROCEDURES ON 2/13/13'''
{| {{table}}
| align="center" style="background:#f0f0f0;"|'''Sample Order'''
| align="center" style="background:#f0f0f0;"|'''PVOH vs. Clay Ratio'''
| align="center" style="background:#f0f0f0;"|'''PVOH Type'''
| align="center" style="background:#f0f0f0;"|'''Clay Selection'''
| align="center" style="background:#f0f0f0;"|'''Amount of Hydrogel Used (g)'''
|-
| 1||50:50||146K||110% CEC Laponite w/ DMHXLBR||0.1081
|-
| 2||50:50||146K||NaMT||0.1221
|-
| 3||50:50||146K||50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||0.1146
|-
| 4||90:10||146K||50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||0.1005
|-
| 5||90:10||146K||NaMT||0.1001
|-
| 6||90:10||146K||110% CEC Laponite w/ DMHXLBR||0.0998
|}
* Specific parameters used to analyze fluorescence of hydrogel samples containing Rhodamine 6G dye included the following:
    # Excitation: 480nm
    # Emission Range: 500-650nm
    # Excitation Slit Width: 10
    # Emission Slit Width: 10
    # Scan Speed: 1200
==Notes==
* As expected, for many of the microsphere placed in the DSC instrument, oil highly affected the analysis of each microsphere sample prepared.
* Many microsphere samples only maintained two data points of information because not enough sample was present for analysis after the safflower oil was cooked off or removed by heat.
* Therefore, it was concluded that DSC would not be a great instrument for analysis of the microspheres especially when not fully dry or encompassed with large amounts of oil.


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Revision as of 09:21, 15 April 2013

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OBJECTIVES

  • Continue fluorescence detection through pressure testing analysis of microsphere samples (new modifications & better results)
  • Continue to run DSC sample analysis on microsphere samples previously prepared on 3/29/13
  • Continue washing with hexanes and drying microspheres prepared on 03/29/13
  • Continue making films containing both clay and PVOH variations to run X-ray analysis

DSC Analysis: Mixed Microspheres 2

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

Sample Name Sample Mass (mg) Pan / Lid Mass (mg)
PVOH 130K 3.01 50.15
PVOH 146K 3.14 49.98
50:50 PVOH 130K NaMT 3.03 49.87
50:50 PVOH 130K Laponite 2.86 49.94
90:10 PVOH 130K 50% CEC NaMT w/ Bu3HdP+ 2.89 50.30
50:50 PVOH 130K 110% CEC NaMT w/ DMHXLBR 3.13 50.55
50:50 PVOH 130K 110% CEC Laponite w/ DMHXLBR 3.17 49.64
90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR 2.89 49.48
50:50 PVOH 130K 50% CEC NaMT w/ Bu3HdP+ 3.04 49.95
  • Specific DSC parameters and protocols set to analyze dry clay samples included the following:
   # Equilibrate sample at ~ -40°C
   # Ramp sample temperature up from 20-240°C
   # Ramp sample temperature down from 20-(-40°C)
   # Repeat segment #2 again

Bent Pipette: Microsphere Pressure Samples Tested

RECALL HYDROGEL PRESSURE TESTING PROTOCOL ON 2/20/13 & FLUORESCENCE ANALYSIS PROCEDURES ON 2/13/13

Sample Order PVOH vs. Clay Ratio PVOH Type Clay Selection Amount of Hydrogel Used (g)
1 50:50 146K 110% CEC Laponite w/ DMHXLBR 0.1081
2 50:50 146K NaMT 0.1221
3 50:50 146K 50% CEC NaMT w/ Bu3HdP+ 0.1146
4 90:10 146K 50% CEC NaMT w/ Bu3HdP+ 0.1005
5 90:10 146K NaMT 0.1001
6 90:10 146K 110% CEC Laponite w/ DMHXLBR 0.0998
  • Specific parameters used to analyze fluorescence of hydrogel samples containing Rhodamine 6G dye included the following:
    # Excitation: 480nm
    # Emission Range: 500-650nm
    # Excitation Slit Width: 10
    # Emission Slit Width: 10
    # Scan Speed: 1200

Notes

  • As expected, for many of the microsphere placed in the DSC instrument, oil highly affected the analysis of each microsphere sample prepared.
  • Many microsphere samples only maintained two data points of information because not enough sample was present for analysis after the safflower oil was cooked off or removed by heat.
  • Therefore, it was concluded that DSC would not be a great instrument for analysis of the microspheres especially when not fully dry or encompassed with large amounts of oil.


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