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

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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 130K3.0150.15
PVOH 146K3.1449.98
50:50 PVOH 130K NaMT3.0349.87
50:50 PVOH 130K Laponite2.8649.94
90:10 PVOH 130K 50% CEC NaMT w/ Bu3HdP+2.8950.30
50:50 PVOH 130K 110% CEC NaMT w/ DMHXLBR3.1350.55
50:50 PVOH 130K 110% CEC Laponite w/ DMHXLBR3.1749.64
90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR2.8949.48
50:50 PVOH 130K 50% CEC NaMT w/ Bu3HdP+3.0449.95
  • 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)
150:50146K110% CEC Laponite w/ DMHXLBR0.1081
250:50146KNaMT0.1221
350:50146K50% CEC NaMT w/ Bu3HdP+0.1146
490:10146K50% CEC NaMT w/ Bu3HdP+0.1005
590:10146KNaMT0.1001
690:10146K110% CEC Laponite w/ DMHXLBR0.0998
  • 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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