User:Karlena L. Brown/Notebook/PVOH Research/2013/02/22

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  • Prepare more microsphere samples expanding upon new previous method developed (new modifications)
  • Continue fluorescence detection through pressure testing analysis of hydrogel samples
  • Run DSC sample analysis on dry clay samples previously prepared on 2/08/13

PVOH 146K Prepared Microsphere Samples & Dye Preparations 3

1μM Rhodamine 6G Dye Concentration (90:10)

  M1V1 = M2V2
  1μM (RG6)x 10mL = (92μM)V2    V2 = 109μL

1μM Rhodamine 6G Dye Concentration (50:50)

  M1V1 = M2V2
  1μM (RG6)x 10mL = (165μM)V2    V2 = 61μL
PVOH vs. Clay Ratio Clay Selection PVOH 146K Mass (g) Actual Clay Mass (g) H2O Added (mL) Dye Concentration (μM) Dye Amount Added (μL)
90:10 50% CEC NaMT w/ Bu3HdP+ 0.90020 0.10330 40 92 109
50:50 50% CEC NaMT w/ Bu3HdP+ 0.50620 0.50090 40 165 61
90:10 NaMT .90160 0.10360 40 92 109


  • 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
  • Originally the type of oil used to prepare microspheres previously was mineral oil; however, safflower oil was used this time as substitute
  • Safflower oil has a higher freezing point than mineral oil
  • 40mL of safflower oil was used and placed in the blender instead of 35mL.
  • Also 40mL of H2O was used to dissolve PVOH clay samples rather than 25mL
  • Once samples placed in 10mL vials after being removed from blender began to settle, each sample was then sonicated before freezing in liquid nitrogen -- keeping microspheres immersed in organic layer
  • Rhodamine 6G dye maintains high affinity for organics; therefore, Rhodamine 6G dye will be added later to each microsphere newly prepared
  • To analyze fluorescence and execute pressure test, hydrogel samples had to be cut into small pieces and smashed up against the glass in order to emulate sheer pressure tests
  • To simulate sheer pressure testing on the hydrogels, Pasteur pipettes were bent at different angles to determine which formation would provide the most sheer pressure and largest fluorescence signal. (Pipette pictures soon to be uploaded)
  • Rather than allowing 20hrs of thawing, microsphere samples will thaw for 12hrs instead
  • Also once fully thawed, each microsphere sample will be sonicated again and frozen in liquid nitrogen before being placed back in freezer