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.
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
X-ray 50-50 130K 110LP micros.png
Figure 2. X-ray diffraction spectrum of PVA 130 microspheres
X-ray diffraction PVA 130 micros.png
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