Objectives
- Finish PVA/clay film preparation.
- Finish preparing DSC samples.
- Run DSC.
- Run X-ray on prepared microspheres with a 50:50 ratio of PVA/clay.
- Add deionized H2O to all prepared hydrogels in preparation for DSC.
- 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 NaMT |
3.10 |
49.78
|
90:10 PVOH 146K NaMT |
3.01 |
49.99
|
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)
|
50:50 |
NaMT |
0.26260 |
0.24770 |
8.0
|
90:10 |
NaMT |
0.40100 |
0.12140 |
8.0
|
50:50 |
Laponite |
0.24750 |
0.24580 |
8.0
|
90:10 |
Laponite |
0.40580 |
0.10910 |
8.0
|
90:10 |
110% CEC Laponite w/ DMHXLBR |
0.25080 |
0.24850 |
8.0
|
50:50 |
110% CEC Laponite w/ DMHXLBR |
0.39820 |
0.10840 |
8.0
|
X-Ray Analysis
|