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

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(Autocreate 2013/04/10 Entry for User:Moira_M._Esson/Notebook/CHEM-581)
Current revision (09:15, 19 April 2013) (view source)
(Film Preparation)
 
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-
==Entry title==
+
==Objectives==
-
* Insert content here...
+
# Make PVOH/clay films in order to run FTIR and X-ray.
 +
# Run both modified and unmodified pressure testing on microspheres with dye added.
 +
# Prepare DSC samples of all decanted and dried microspheres.
 +
<br>
 +
==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 [[User:Moira_M._Esson/Notebook/CHEM-581/2012/08/29|2012/08/29]] was used
 +
<br>
 +
Table 1. Film Preparation
 +
<br>
 +
 
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''PVOH vs. Clay Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''Clay Selection'''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH 130K Mass (g)'''
 +
| align="center" style="background:#f0f0f0;"|'''Actual Clay Mass (g)'''
 +
| align="center" style="background:#f0f0f0;"|'''H<sub>2</sub>O Added (mL)'''
 +
|-
 +
| NONE||NONE||0.49990||NONE||8.0
 +
|-
 +
| 50:50||50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||0.25280||0.2468||8.0
 +
|-
 +
| 90:10||50% CEC NaMT||0.45770||0.05030||8.0
 +
|-
 +
| 50:50||110% CEC NaMT||0.25020||0.25010||8.0
 +
|-
 +
| 90:10||110% CEC NaMT||0.45020||0.05240||8.0
 +
|}
 +
 
 +
<br>
 +
*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
 +
<br>
 +
 
 +
==Pressure Testing==
 +
*The unmodified pipette pressure testing samples of Rhodamine 6G obtained on [[User:Moira_M._Esson/Notebook/CHEM-581/2013/04/05|2013/04/05]] were run on the fluorimeter.
 +
*The specific parameters used for analysis of the fluorescence of Rhodamine 6G released from clay incorporated microspheres included:
 +
    # Excitation: 480nm
 +
    # Emission Range: 500-650nm
 +
    # Excitation Slit Width: 10
 +
    # Emission Slit Width: 10
 +
    # Scan Speed: 1200
 +
<br>
 +
Figure 1. Fluorescence of Rhodamine 6G in water collected from pressure testing of PVA/clay microspheres using an unmodified pipette
 +
<br>
 +
[[Image:Pressure testing of micros146K unmodpipette.png]]
 +
<br>
 +
*Only the 90:10 PVA146:110% LP produced a clean peak.
 +
*50:50PVA146:110%LP produced the highest fluorescence intensity value.
 +
<br>
 +
 
 +
Figure 2. Fluorescence of Rhodamine 6G in water collected from pressure testing of PVA/clay microspheres using a modified pipette
 +
<br>
 +
[[Image:Pressure testingmicros146modifpipette.png]]
 +
<br>
 +
*50:50 PVA146K:110%LP produced the highest fluorescence intensity value
 +
'''Modified Pipette Pressure Testing'''
 +
<br>
 +
*The general protocol for modified pipette pressure testing on hydrogels described on [[User:Moira_M._Esson/Notebook/CHEM-581/2013*The specific parameters used for analysis of the fluorescence of Rhodamine 6G released from clay incorporated microspheres included:
 +
    # Excitation: 480nm
 +
    # Emission Range: 500-650nm
 +
    # Excitation Slit Width: 10
 +
    # Emission Slit Width: 10
 +
    # Scan Speed: 1200
 +
<br> 
 +
Table 2. Samples used for Modified pressure testing
 +
<br>
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Sample Order'''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH vs. Clay Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH Type'''
 +
| align="center" style="background:#f0f0f0;"|'''Clay Selection'''
 +
| align="center" style="background:#f0f0f0;"|'''Amount of Hydrogel Used (g)'''
 +
|-
 +
| 1||50:50||146K||110% CEC Laponite w/ DMHXLBR||0.1081
 +
|-
 +
| 2||50:50||146K||NaMT||0.1221
 +
|-
 +
| 3||50:50||146K||50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||0.1146
 +
|-
 +
| 4||90:10||146K||50% CEC NaMT w/ Bu<sub>3</sub>HdP<sup>+</sup>||0.1005
 +
|-
 +
| 5||90:10||146K||NaMT||0.1001
 +
|-
 +
| 6||90:10||146K||110% CEC Laponite w/ DMHXLBR||0.0998
 +
|}
 +
 
 +
<br>
 +
 
 +
==DSC Analysis==
 +
*The general protocol for DSC analysis was followed.
 +
* Specific DSC parameters ato analyze the following PVA/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
 +
 
 +
Table 3. DSC samples information
 +
<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)'''
 +
|-
 +
| PVOH 130K||3.01||50.15
 +
|-
 +
| 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
 +
|}
 +
<br>
 +
*The following data samples will be collected during the next session.
 +
*Any previously run samples that were unable to be analyzed(described [[User:Moira_M._Esson/Notebook/CHEM-581/2013/04/05|2013/04/05]] were also re-run and will be collected during the next session.
 +
 
 +
==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.
 +
 
 +
 

Current revision

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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 130K 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 samples of Rhodamine 6G obtained on 2013/04/05 were run on the fluorimeter.
  • The specific parameters used for analysis of the fluorescence of Rhodamine 6G released from clay incorporated microspheres included:
    # Excitation: 480nm
    # Emission Range: 500-650nm
    # Excitation Slit Width: 10
    # Emission Slit Width: 10
    # Scan Speed: 1200 


Figure 1. Fluorescence of Rhodamine 6G in water collected from pressure testing of PVA/clay microspheres using an unmodified pipette
Image:Pressure testing of micros146K unmodpipette.png

  • Only the 90:10 PVA146:110% LP produced a clean peak.
  • 50:50PVA146:110%LP produced the highest fluorescence intensity value.


Figure 2. Fluorescence of Rhodamine 6G in water collected from pressure testing of PVA/clay microspheres using a modified pipette
Image:Pressure testingmicros146modifpipette.png

  • 50:50 PVA146K:110%LP produced the highest fluorescence intensity value

Modified Pipette Pressure Testing

  • The general protocol for modified pipette pressure testing on hydrogels described on [[User:Moira_M._Esson/Notebook/CHEM-581/2013*The specific parameters used for analysis of the fluorescence of Rhodamine 6G released from clay incorporated microspheres included:
    # Excitation: 480nm
    # Emission Range: 500-650nm
    # Excitation Slit Width: 10
    # Emission Slit Width: 10
    # Scan Speed: 1200 


Table 2. Samples used for Modified pressure testing

Sample Order PVOH vs. Clay Ratio PVOH Type Clay Selection Amount of Hydrogel Used (g)
150:50146K110% CEC Laponite w/ DMHXLBR0.1081
250:50146KNaMT0.1221
350:50146K50% CEC NaMT w/ Bu3HdP+0.1146
490:10146K50% CEC NaMT w/ Bu3HdP+0.1005
590:10146KNaMT0.1001
690:10146K110% CEC Laponite w/ DMHXLBR0.0998


DSC Analysis

  • The general protocol for DSC analysis was followed.
  • Specific DSC parameters ato analyze the following PVA/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

Table 3. DSC samples information

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


  • The following data samples will be collected during the next session.
  • Any previously run samples that were unable to be analyzed(described 2013/04/05 were also re-run and will be collected during the next session.

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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