User:Moira M. Esson/Notebook/CHEM-581/2013/04/12

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==X-Ray Analysis==

Revision as of 12:12, 15 April 2013

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Objectives

  1. Finish PVA/clay film preparation.
  2. Finish preparing DSC samples.
  3. Run DSC.
  4. Run X-ray on prepared microspheres with a 50:50 ratio of PVA/clay.
  5. Add deionized H2O to all prepared hydrogels in preparation for DSC.
  6. View prepared microspheres under microscope.


DSC

  • The general protocol for DSC was used
  • Specific DSC parameters and protocols set to analyze PVA/clay samples were:
   # 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


Table 1. DSC sample preparation

Sample Name Sample Mass (mg) Pan / Lid Mass (mg)
90:10 PVOH 146K 50% CEC NaMT3.1049.78
90:10 PVOH 146K NaMT3.0149.99


Film Preparation

  • The general protocol for film preparation described on 2012/08/29 was followed. The necessary amount of clay was added in the correct ratio. All films were prepared on a 0.5g scale. The films were placed in a freezer at -20°C immediately after pouring. These films will undergo the cyclic freeze-thaw procedure used for hydrogel preparation.


Table 2. Film Preparation

PVOH vs. Clay Ratio Clay Selection PVOH 146K Mass (g) Actual Clay Mass (g) H2O Added (mL)
50:50NaMT0.262600.247708.0
90:10NaMT0.401000.121408.0
50:50Laponite0.247500.245808.0
90:10Laponite0.405800.109108.0
90:10110% CEC Laponite w/ DMHXLBR0.250800.248508.0
50:50110% CEC Laponite w/ DMHXLBR0.398200.108408.0


X-Ray Analysis


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