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

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  • 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


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


  • 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.