User:Moira M. Esson/Notebook/CHEM-581/2013/04/10

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(Notes)
(Film Preparation)
Line 41: Line 41:
*After they were placed in the freezer, frost appear to cover the films and they appeared to shrink in comparison to the hydrogels which expanded upon freezing
*After they were placed in the freezer, frost appear to cover the films and they appeared to shrink in comparison to the hydrogels which expanded upon freezing
<br>
<br>
 +
==Pressure Testing==
 +
*The unmodified pipette pressure testing obtained on [[User:Moira_M._Esson/Notebook/CHEM-581/2013/04/05|2013/04/05]]
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<br>
 +
==DSC Analysis==
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 +
{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Sample Name'''
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| align="center" style="background:#f0f0f0;"|'''Sample Mass (mg)'''
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| align="center" style="background:#f0f0f0;"|'''Pan / Lid Mass (mg)'''
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|-
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| PVOH 130K||3.01||50.15
 +
|-
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| PVOH 146K||3.14||49.98
 +
|-
 +
| 50:50 PVOH 130K NaMT||3.03||49.87
 +
|-
 +
| 50:50 PVOH 130K Laponite||2.86||49.94
 +
|-
 +
| 90:10 PVOH 130K 50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||2.89||50.30
 +
|-
 +
| 50:50 PVOH 130K 110% CEC NaMT w/ DMHXLBR||3.13||50.55
 +
|-
 +
| 50:50 PVOH 130K 110% CEC Laponite w/ DMHXLBR||3.17||49.64
 +
|-
 +
| 90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR||2.89||49.48
 +
|-
 +
| 50:50 PVOH 130K 50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||3.04||49.95
 +
|}
 +
 +
* Specific DSC parameters and protocols set to analyze dry clay samples included the following:
 +
    # Equilibrate sample at ~ -40°C
 +
    # Ramp sample temperature up from 20-240°C
 +
    # Ramp sample temperature down from 20-(-40°C)
 +
    # Repeat segment #2 again
 +
==Notes==
==Notes==
* As expected, for many of the microsphere placed in the DSC instrument, oil highly affected the analysis of each microsphere sample prepared. Although it was anticipated that a large oil contamination peak would appear, almost all of the microsphere samples only contained two data sample points. DSC will be run again in order to test whether DSC will be able to be used.
* As expected, for many of the microsphere placed in the DSC instrument, oil highly affected the analysis of each microsphere sample prepared. Although it was anticipated that a large oil contamination peak would appear, almost all of the microsphere samples only contained two data sample points. DSC will be run again in order to test whether DSC will be able to be used.

Revision as of 09:38, 15 April 2013

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Objectives

  1. Make PVOH/clay films in order to run FTIR and X-ray.
  2. Run both modified and unmodified pressure testing on microspheres with dye added.
  3. Prepare DSC samples of all decanted and dried microspheres.


Film Preparation

  • PVA/clay films were prepared in order to run examine these films using FTIR and X-ray. These films will be compared to the hydrogel and microsphere samples in order to determine the difference between the prepared PVA/clay structures.
  • The films were prepared using the same PVA/clay ratio as that of the prepared microspheres and hydrogels.
  • The General Protocol for PVOH film preparation described on 2012/08/29 was used


Table 1. Film Preparation

PVOH vs. Clay Ratio Clay Selection PVOH 146K Mass (g) Actual Clay Mass (g) H2O Added (mL)
NONENONE0.49990NONE8.0
50:5050% CEC NaMT w/ Bu3HdP+0.252800.24688.0
90:1050% CEC NaMT0.457700.050308.0
50:50110% CEC NaMT0.250200.250108.0
90:10110% CEC NaMT0.450200.052408.0


  • After being poured into the Teflon dish, these films were placed in a freezer at -20°C. These films will undergo the same, 3 day freeze-thaw method that both the microspheres and hydrogels were subjected to.
  • After they were placed in the freezer, frost appear to cover the films and they appeared to shrink in comparison to the hydrogels which expanded upon freezing


Pressure Testing

  • The unmodified pipette pressure testing obtained on 2013/04/05


DSC Analysis

Sample Name Sample Mass (mg) Pan / Lid Mass (mg)
PVOH 130K3.0150.15
PVOH 146K3.1449.98
50:50 PVOH 130K NaMT3.0349.87
50:50 PVOH 130K Laponite2.8649.94
90:10 PVOH 130K 50% CEC NaMT w/ Bu3HdP+2.8950.30
50:50 PVOH 130K 110% CEC NaMT w/ DMHXLBR3.1350.55
50:50 PVOH 130K 110% CEC Laponite w/ DMHXLBR3.1749.64
90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR2.8949.48
50:50 PVOH 130K 50% CEC NaMT w/ Bu3HdP+3.0449.95
  • Specific DSC parameters and protocols set to analyze dry clay samples included the following:
   # Equilibrate sample at ~ -40°C
   # Ramp sample temperature up from 20-240°C
   # Ramp sample temperature down from 20-(-40°C)
   # Repeat segment #2 again

Notes

  • As expected, for many of the microsphere placed in the DSC instrument, oil highly affected the analysis of each microsphere sample prepared. Although it was anticipated that a large oil contamination peak would appear, almost all of the microsphere samples only contained two data sample points. DSC will be run again in order to test whether DSC will be able to be used.




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