OBJECTIVES
- 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
RECALL HYDROGEL PRESSURE TESTING PROTOCOL ON 2/20/13 & FLUORESCENCE ANALYSIS PROCEDURES ON 2/13/13
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
Notes
- 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.
|