User:Moira M. Esson/Notebook/CHEM-581/2013/04/03: Difference between revisions

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*It was found that the organic safflower oil layer needed to be removed several times. After removing a layer of safflower oil, the microspheres were allowed to sit for 15 minutes, and more oil was then able to be removed.
*It was found that the organic safflower oil layer needed to be removed several times. After removing a layer of safflower oil, the microspheres were allowed to sit for 15 minutes, and more oil was then able to be removed.
*Due to the presence of what appeared to be small particles in the safflower oil, the safflower oil layer that was removed from the samples was saved, labeled and parafilmed. The safflower oil layer will be vacuum filtered and obtained solids will be tested using DSC in order to see if there is a difference between the larger spheres that formed at the bottom of the vial and the smaller particles suspended in the safflower oil layer.
*Due to the presence of what appeared to be small particles in the safflower oil, the safflower oil layer that was removed from the samples was saved, labeled and parafilmed. The safflower oil layer will be vacuum filtered and obtained solids will be tested using DSC in order to see if there is a difference between the larger spheres that formed at the bottom of the vial and the smaller particles suspended in the safflower oil layer.
<br>
==DSC==
*Please refer to Karlena Brown's laboratory notebook [[User:Karlena_L._Brown/Notebook/PVOH_Research/2013/04/03|2013/04/03]] for any information concerning DSC sample preparation.
* For many of the DSC samples run, the microsphere samples analyzed were not completely dry. As such, the DSC peak analysis will be affected by the presence of safflower oil encompassed in the sample
* X-ray diffraction will be run on all prepared microsphere samples in order to determine whether clay has agglomerated separately from the PVOH
<br>
'''DSC samples''':
<br>
{| {{table}}
| align="center" style="background:#f0f0f0;"|'''Sample Name'''
| align="center" style="background:#f0f0f0;"|'''Sample Mass (mg)'''
| align="center" style="background:#f0f0f0;"|'''Pan / Lid Mass (mg)'''
|-
| 50:50 PVOH 130K NaMT||3.12||50.01
|-
| 90:10 PVOH 130K 110% CEC NaMT w/ DMHXLBR||2.29||50.17
|-
| 90:10 PVOH 130K Laponite||2.59||50.12
|-
| 90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR||2.27||50.28
|-
| 90:10 PVOH 146K 110% CEC NaMT w/ DMHXLBR||2.65||50.11
|-
| 50:50 PVOH 146K 110% CEC NaMT w/ DMHXLBR||2.50||50.17
|}
<br>
'''DSC Data Collection'''
Figure 1. DSC graph of 50% CEC NaMT clay with Bu<sub>3</sub>HdP<sup>+</sup> surfactant
<br>
[[Image:50% CEC NAMT.jpg|400px]]
<br>
Figure 2. DSC graph of 110% CEC Laponite clay with DMHXLBr surfactant
<br>
[[Image:110 LP DMHXLBR.png|500px]]
<br>
Figure 3. DSC graph of 110% CEC NaMT clay with DMHXLBr surfactant
<br>
[[Image:110 NaMT DMHXLBR.png|500px]]
<br>
Figure 4. DSC graph of Laponite clay
<br>
[[Image:Laponite.png|500px]]
<br>
Figure 5. DSC graph of NaMT clay
<br>
[[Image:NaMT.png|500px]]
<br>
Figure 6. DSC graph of microspheres prepared with a 90:10 ratio of PVA MW 146,000-186,000:Laponite clay
<br>
[[Image:90-10 146K LP.png|500px]]
<br>
==Diffusion Testing==
A new general protocol for the preparation of was used for the diffusion testing of the prepared microspheres. It was determined that the previous protocol did not allow for a quantitative understanding of the amount of dye diffused from the samples.
<br>
'''General Protocol''':
# The microspheres were removed from their respective vial and placed in new, clean 20mL vials.
# 15mL of deionized H<sub>2</sub>O were added to each vial.
# A timer was started, and every 15 minutes, a sample of distilled H<sub>2</sub>O was removed from the beaker and placed in an unfrosted cuvette.
# After running the sample on the fluorimeter, the sample was readded to the diffusion vial.
# This process was repeated for 2 hours.
<br>
'''General information on the parameters of the fluorescence run''':
#Starting wavelength: 500nm
#End wavelength: 650nm
#Excitation wavelength: 526nm
#Exitation slit: 10
#Emission slit: 10
#Scan rate/Speed: 1200
<br>
'''Spectra'''
<br>
Figure 7. Diffusion Testing of Rhodamine 6G in microspheres prepared with 90:10 ratio of PVA MW 146,000-186,000: 50% CEC NaMT
<br>
[[Image:90 pva 146 50NaMT micros diffusion.jpg]]
<br>
*Fluorescence intensity maximum is 6.985.
<br>
Figure 8. Diffusion Testing of Rhodamine 6G in microspheres prepared with 90:10 ratio of PVA MW 146,000-186,000: 110% Laponite
<br>
[[Image:90 PVA 146 110LP micros diff.jpg]]
<br>
*Fluorescence intensity maximum is 5.109.
<br>
Figure 9. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 90:10 ratio PVA 146,000-186,000: NaMT
<br>
[[Image:90 PVA 146 NaMT micros diff test.png]]
<br>  
<br>  
==Diffusion Testing==
*Fluorescence intensity maximum is 26.734
<br>
Figure 10. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: NaMT
<br>
[[Image:50 PVA 146 NaMT micros diff.png]]
*Fluorescence intensity maximum is 16.350
<br>
Figure 11. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: 50% CEC NaMT
<br>
[[Image:50 PVA 146 50NaMT micros diff.png]]
<br>
*Fluorescence intensity maximum is 11.661
<br>
Figure 12. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: 110% CEC Laponite
<br>
[[Image:50 PVA 146 110 LP.png]]
<br>
*Fluorescence intensity maximum is 137.319.
<br>
 
==Notes==
* The tested "microspheres" more closely resemble smaller, more circular, more flexible hydrogels. Other microsphere samples were prepared and may more closely resemble microspheres.
* The microsphere prepared with a 50:50 ratio PVA 146,000-186,000: 110% CEC Laponite caused the most diffusion of dye. All microspheres will be used for pressure testing, however, because not all dye leaked out.
* All curves will be integrated in order to determine the concentration of dye leaked.
   
   


Revision as of 06:58, 15 April 2013

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Objectives

  • Run diffusion testing on microspheres with dye added 2013/03/20. These microspheres were prepared on 2013/02/20.
  • Run DSC of microsphere samples prepared on 2013/03/22
  • Decant microsphere samples prepared on 2013/03/29

Decanting

The general protocol described on 2013/03/01 was followed.

  • It was found that the organic safflower oil layer needed to be removed several times. After removing a layer of safflower oil, the microspheres were allowed to sit for 15 minutes, and more oil was then able to be removed.
  • Due to the presence of what appeared to be small particles in the safflower oil, the safflower oil layer that was removed from the samples was saved, labeled and parafilmed. The safflower oil layer will be vacuum filtered and obtained solids will be tested using DSC in order to see if there is a difference between the larger spheres that formed at the bottom of the vial and the smaller particles suspended in the safflower oil layer.


DSC

  • Please refer to Karlena Brown's laboratory notebook 2013/04/03 for any information concerning DSC sample preparation.
  • For many of the DSC samples run, the microsphere samples analyzed were not completely dry. As such, the DSC peak analysis will be affected by the presence of safflower oil encompassed in the sample
  • X-ray diffraction will be run on all prepared microsphere samples in order to determine whether clay has agglomerated separately from the PVOH


DSC samples:

Sample Name Sample Mass (mg) Pan / Lid Mass (mg)
50:50 PVOH 130K NaMT 3.12 50.01
90:10 PVOH 130K 110% CEC NaMT w/ DMHXLBR 2.29 50.17
90:10 PVOH 130K Laponite 2.59 50.12
90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR 2.27 50.28
90:10 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.65 50.11
50:50 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.50 50.17


DSC Data Collection Figure 1. DSC graph of 50% CEC NaMT clay with Bu3HdP+ surfactant

Figure 2. DSC graph of 110% CEC Laponite clay with DMHXLBr surfactant

Figure 3. DSC graph of 110% CEC NaMT clay with DMHXLBr surfactant

Figure 4. DSC graph of Laponite clay

Figure 5. DSC graph of NaMT clay

Figure 6. DSC graph of microspheres prepared with a 90:10 ratio of PVA MW 146,000-186,000:Laponite clay

Diffusion Testing

A new general protocol for the preparation of was used for the diffusion testing of the prepared microspheres. It was determined that the previous protocol did not allow for a quantitative understanding of the amount of dye diffused from the samples.
General Protocol:

  1. The microspheres were removed from their respective vial and placed in new, clean 20mL vials.
  2. 15mL of deionized H2O were added to each vial.
  3. A timer was started, and every 15 minutes, a sample of distilled H2O was removed from the beaker and placed in an unfrosted cuvette.
  4. After running the sample on the fluorimeter, the sample was readded to the diffusion vial.
  5. This process was repeated for 2 hours.


General information on the parameters of the fluorescence run:

  1. Starting wavelength: 500nm
  2. End wavelength: 650nm
  3. Excitation wavelength: 526nm
  4. Exitation slit: 10
  5. Emission slit: 10
  6. Scan rate/Speed: 1200


Spectra
Figure 7. Diffusion Testing of Rhodamine 6G in microspheres prepared with 90:10 ratio of PVA MW 146,000-186,000: 50% CEC NaMT

  • Fluorescence intensity maximum is 6.985.


Figure 8. Diffusion Testing of Rhodamine 6G in microspheres prepared with 90:10 ratio of PVA MW 146,000-186,000: 110% Laponite

  • Fluorescence intensity maximum is 5.109.


Figure 9. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 90:10 ratio PVA 146,000-186,000: NaMT

  • Fluorescence intensity maximum is 26.734


Figure 10. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: NaMT

  • Fluorescence intensity maximum is 16.350


Figure 11. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: 50% CEC NaMT

  • Fluorescence intensity maximum is 11.661


Figure 12. Diffusion Testing of Rhodamine 6G in microspheres prepared with a 50:50 ratio PVA 146,000-186,000: 110% CEC Laponite

  • Fluorescence intensity maximum is 137.319.


Notes

  • The tested "microspheres" more closely resemble smaller, more circular, more flexible hydrogels. Other microsphere samples were prepared and may more closely resemble microspheres.
  • The microsphere prepared with a 50:50 ratio PVA 146,000-186,000: 110% CEC Laponite caused the most diffusion of dye. All microspheres will be used for pressure testing, however, because not all dye leaked out.
  • All curves will be integrated in order to determine the concentration of dye leaked.



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