Objectives
- Perform pressure testing of microspheres.
- Run X-ray diffraction on a plain safflower oil sample, a plain PVA MW 130 sample, and a PVA 146 microsphere sample that ended up becoming a hydrogel.
- Finish running DSC on a Rhodamine 6G sample(this was unable to be run last time due to lack of gas).
Pressure Testing
- The general protocol for pressure testing described on 2013/04/17 was followed.
Figure 1. Pressure testing of prepared microspheres.
- It appears as if these microspheres exhibit some sheer pressure response due to the presence of a slight R6G peak.
X-ray
General Protocol:
- Use a Kimwipe and acetone to thoroughly clean the low background sample holder
- Insert Sample into the low background holder. Note: Must make sure that the sample is completely flat and that the particle sample size is very small. If the sample is too large, use a mortar and pestle to completely grind the sample
- Turn on the chiller
- Turn on Miniflex II. This is the white button on the machine
- Turn on X-ray. The machine will be on when the red lights on the button labeled x-ray light up
- Using a Geiger counter, test the radiation from the machine
- Set sample in sample holder and record sample holder number
- Close the door to the x-ray
- Open software on computer
Figure 1. X-ray diffraction spectrum of a 50:50 ratio PVA130:110% Laponite
Figure 2. X-ray diffraction spectrum of PVA 130 microspheres
Table 1. All X-ray data
| '
|
2Ѳ (degree)
|
'
|
'
|
'
|
'
|
| Sample Name |
Peak 1 |
Peak 2 |
Peak 3 |
Peak 4 |
Peak 5
|
| NaMT |
7.33 |
19.77 |
28.52 |
35.16 |
|
| Laponite |
6.92 |
19.70 |
27.90 |
35.30 |
|
| 110% CEC NaMT w/ DMHXLBR |
6.76 |
19.98 |
27.27 |
|
|
| 110% CEC Laponite w/ DMHXLBR |
6.61 |
19.79 |
27.10 |
35.28 |
|
| PVA 130K Film |
4.33 |
2.16 |
|
|
|
| PVA 130K Microspheres |
4.52 |
19.82 |
|
|
|
| 50:50 PVA 130K NaMT Film |
3.27 |
20.43 |
26.61 |
|
|
| 50:50 PVA 130K NaMT Microspheres |
4.42 |
19.71 |
|
|
|
| 50:50 PVA 130K 110% NaMT Film |
2.39 |
5.53 |
9.68 |
19.71 |
27.27
|
| 50:50 PVA 130K 110% NaMT Microspheres |
19.56 |
|
|
|
|
| 50:50 PVA 130K Laponite Film |
3.72 |
4.44 |
|
|
|
| 50:50 PVA 130K Laponite Microspheres |
19.87 |
|
|
|
|
| 50:50 PVA 130K 110% Laponite Film |
6.49 |
19.57 |
|
|
|
| 50:50 PVA 130K 110% Laponite Microspheres |
19.45 |
|
|
|
|
Table 2. All X-ray data continued
| '
|
D spacing
|
'
|
'
|
'
|
'
|
| Sample Name |
Peak 1 |
Peak 2 |
Peak 3 |
Peak 4 |
Peak 5
|
| NaMT |
12.05 |
4.48 |
3.13 |
2.55 |
|
| Laponite |
12.76 |
4.50 |
3.19 |
2.54 |
|
| 110% CEC NaMT w/ DMHXLBR |
13.06 |
4.44 |
3.27 |
|
|
| 110% CEC Laponite w/ DMHXLBR |
13.37 |
4.48 |
3.29 |
2.54 |
|
| PVA 130K Film |
20.48 |
41.74 |
|
|
|
| PVA 130K Microspheres |
19.50 |
4.48 |
|
|
|
| 50:50 PVA 130K NaMT Film |
26.97 |
4.34 |
3.35 |
|
|
| 50:50 PVA 130K NaMT Microspheres |
20.00 |
4.50 |
|
|
|
| 50:50 PVA 130K 110% NaMT Film |
36.90 |
16.00 |
9.13 |
4.50 |
3.27
|
| 50:50 PVA 130K 110% NaMT Microspheres |
4.53 |
|
|
|
|
| 50:50 PVA 130K Laponite Film |
23.70 |
20.00 |
|
|
|
| 50:50 PVA 130K Laponite Microspheres |
4.46 |
|
|
|
|
| 50:50 PVA 130K 110% Laponite Film |
13.60 |
4.53 |
|
|
|
| 50:50 PVA 130K 110% Laponite Microspheres |
4.56 |
|
|
|
|
|
Project name
