User:Moira M. Esson/Notebook/CHEM-581/2013/04/19

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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.
Image:Pressure test micros.png

  • It appears as if these microspheres exhibit some sheer pressure response due to the presence of a slight R6G peak.

X-ray

General Protocol:

  1. Use a Kimwipe and acetone to thoroughly clean the low background sample holder
  2. 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
  3. Turn on the chiller
  4. Turn on Miniflex II. This is the white button on the machine
  5. Turn on X-ray. The machine will be on when the red lights on the button labeled x-ray light up
  6. Using a Geiger counter, test the radiation from the machine
  7. Set sample in sample holder and record sample holder number
  8. Close the door to the x-ray
  9. Open software on computer


Figure 1. X-ray diffraction spectrum of a 50:50 ratio PVA130:110% Laponite
Image:X-ray 50-50 130K 110LP micros.png
Figure 2. X-ray diffraction spectrum of PVA 130 microspheres
Image:X-ray diffraction PVA 130 micros.png
Table 1. All X-ray data

' 2Ѳ (degree) ' ' ' '
Sample NamePeak 1Peak 2Peak 3Peak 4Peak 5
NaMT7.3319.7728.5235.16
Laponite6.9219.7027.9035.30
110% CEC NaMT w/ DMHXLBR6.7619.9827.27
110% CEC Laponite w/ DMHXLBR6.6119.7927.1035.28
PVA 130K Film4.332.16
PVA 130K Microspheres4.5219.82
50:50 PVA 130K NaMT Film3.2720.4326.61
50:50 PVA 130K NaMT Microspheres4.4219.71
50:50 PVA 130K 110% NaMT Film2.395.539.6819.7127.27
50:50 PVA 130K 110% NaMT Microspheres19.56
50:50 PVA 130K Laponite Film3.724.44
50:50 PVA 130K Laponite Microspheres19.87
50:50 PVA 130K 110% Laponite Film6.4919.57
50:50 PVA 130K 110% Laponite Microspheres19.45


Table 2. All X-ray data continued

' D spacing ' ' ' '
Sample NamePeak 1Peak 2Peak 3Peak 4Peak 5
NaMT12.054.483.132.55
Laponite12.764.503.192.54
110% CEC NaMT w/ DMHXLBR13.064.443.27
110% CEC Laponite w/ DMHXLBR13.374.483.292.54
PVA 130K Film20.4841.74
PVA 130K Microspheres19.504.48
50:50 PVA 130K NaMT Film26.974.343.35
50:50 PVA 130K NaMT Microspheres20.004.50
50:50 PVA 130K 110% NaMT Film36.9016.009.134.503.27
50:50 PVA 130K 110% NaMT Microspheres4.53
50:50 PVA 130K Laponite Film23.7020.00
50:50 PVA 130K Laponite Microspheres4.46
50:50 PVA 130K 110% Laponite Film13.604.53
50:50 PVA 130K 110% Laponite Microspheres4.56



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