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

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(X-ray)
Current revision (17:30, 27 April 2013) (view source)
(X-ray)
 
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[[Image:Pressure test micros.png]]
[[Image:Pressure test micros.png]]
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* It appears as if these microspheres exhibit some sheer pressure response due to the presence of a slight R6G peak.
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==X-ray==
==X-ray==
General Protocol:
General Protocol:
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# Open software on computer  
# Open software on computer  
<br>
<br>
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*The samples will be posted when received.
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Figure 1. X-ray diffraction spectrum of a 50:50 ratio PVA130:110% Laponite
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<br>
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[[Image:X-ray 50-50 130K 110LP micros.png]]
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<br>
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Figure 2. X-ray diffraction spectrum of PVA 130 microspheres
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<br>
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[[Image:X-ray diffraction PVA 130 micros.png]]
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<br>
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Table 1. All X-ray data
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<br>
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|'''2Ѳ (degree)'''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Sample Name||Peak 1||Peak 2||Peak 3||Peak 4||Peak 5
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|-
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| NaMT||7.33||19.77||28.52||35.16||
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|-
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| Laponite||6.92||19.70||27.90||35.30||
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|-
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| 110% CEC NaMT w/ DMHXLBR||6.76||19.98||27.27||||
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|-
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| 110% CEC Laponite w/ DMHXLBR||6.61||19.79||27.10||35.28||
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|-
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| PVA 130K Film||4.33||2.16||||||
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|-
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| PVA 130K Microspheres||4.52||19.82||||||
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|-
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| 50:50 PVA 130K NaMT Film||3.27||20.43||26.61||||
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|-
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| 50:50 PVA 130K NaMT Microspheres||4.42||19.71||||||
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|-
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| 50:50 PVA 130K 110% NaMT Film||2.39||5.53||9.68||19.71||27.27
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|-
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| 50:50 PVA 130K 110% NaMT Microspheres||19.56||||||||
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|-
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| 50:50 PVA 130K Laponite Film||3.72||4.44||||||
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|-
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| 50:50 PVA 130K Laponite Microspheres||19.87||||||||
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|-
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| 50:50 PVA 130K 110% Laponite Film||6.49||19.57||||||
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|-
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| 50:50 PVA 130K 110% Laponite Microspheres||19.45||||||||
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|-
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|}
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<br>
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Table 2. All X-ray data continued
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<br>
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|'''D spacing'''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Sample Name||Peak 1||Peak 2||Peak 3||Peak 4||Peak 5
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|-
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| NaMT||12.05||4.48||3.13||2.55||
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|-
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| Laponite||12.76||4.50||3.19||2.54||
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|-
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| 110% CEC NaMT w/ DMHXLBR||13.06||4.44||3.27||||
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|-
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| 110% CEC Laponite w/ DMHXLBR||13.37||4.48||3.29||2.54||
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|-
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| PVA 130K Film||20.48||41.74||||||
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|-
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| PVA 130K Microspheres||19.50||4.48||||||
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|-
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| 50:50 PVA 130K NaMT Film||26.97||4.34||3.35||||
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|-
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| 50:50 PVA 130K NaMT Microspheres||20.00||4.50||||||
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|-
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| 50:50 PVA 130K 110% NaMT Film||36.90||16.00||9.13||4.50||3.27
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|-
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| 50:50 PVA 130K 110% NaMT Microspheres||4.53||||||||
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|-
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| 50:50 PVA 130K Laponite Film||23.70||20.00||||||
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|-
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| 50:50 PVA 130K Laponite Microspheres||4.46||||||||
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|-
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| 50:50 PVA 130K 110% Laponite Film||13.60||4.53||||||
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|-
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| 50:50 PVA 130K 110% Laponite Microspheres||4.56||||||||
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|}

Current revision

Project name Main project page
Previous entry      

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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