User:Karlena L. Brown/Notebook/PVOH Research/2013/04/03

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OBJECTIVES

  • Collect all DSC results from dry clay samples previously prepared on 2/08/13
  • Run DSC sample analysis on dry clay samples previously prepared on 3/29/13
  • Remove all excess oil from controlled microsphere samples prepared on 03/29/13
  • Run fluorescence analysis on all microsphere samples prepared 02/20/13 with Rhodamine 6G dye

DSC Results for Dry Clay Samples

DSC Analysis: Mixed Microspheres

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)
50:50 PVOH 130K NaMT 3.12 50.01
90:10 PVOH 130K 110% CEC NaMT w/ DMHXLBR 2.29 50.17
90:10 PVOH 130K Laponite 2.59 50.12
90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR 2.27 50.28
90:10 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.65 50.11
50:50 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.50 50.17
  • 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

Fluorescence Analysis: Diffusion Testing 2

RECALL DIFFUSION TESTING PROTOCOL ON 2/15/13

  • Fluorescent samples run and completed for 2hr diffusion rate determinations:
  # Microsphere 90:10 PVOH 146K 50% CEC NaMT w/ Bu3HdP+
  # Microsphere 90:10 PVOH 146K 110% CEC Laponite w/ DMHXLBR
  # Microsphere 90:10 PVOH 146K NaMT
  # Microsphere 50:50 PVOH 146K NaMT
  # Microsphere 50:50 PVOH 146K 50% CEC NaMT w/ Bu3HdP+
  # Microsphere 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR
  • 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

Fluorescence Results & Spectrums


Figure 1 - Microsphere 90:10 PVOH 146K 50% CEC NaMT w/ Bu3HdP+

***Fluorescence intensity maximum is 6.985


Figure 2 - Microsphere 90:10 PVOH 146K 110% CEC Laponite w/ DMHXLBR

***Fluorescence intensity maximum is 5.109


Figure 3 - Microsphere 90:10 PVOH 146K NaMT

***Fluorescence intensity maximum is 26.734


Figure 4 - Microsphere 50:50 PVOH 146K NaMT
***Fluorescence intensity maximum is 17.


Figure 5 - Microsphere 50:50 PVOH 146K 50% CEC NaMT w/ Bu3HdP+

***Fluorescence intensity maximum is 11.661


Figure 6 - Microsphere 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR

***Fluorescence intensity maximum is 137.319

Notes

  • For many of the DSC samples run, the microsphere samples analyzed were not completely dry; therefore, the DSC peak analysis will be highly affected by the presence of safflower oil encompassed in the sample
  • X-ray diffraction will be run on all prepared microsphere samples in order to determine whether clay has agglomerated separately from the PVOH
  • For hydrophilic polymers blended with clay, it was referenced that a peak shift below 10° was a strong indicator of excellent conglomeration
  • The microsphere prepared with 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR caused the most diffusion of dye
  • All microspheres will be used for pressure testing, however, because not all dye leaked out