User:Moira M. Esson/Notebook/CHEM-581/2013/04/12: Difference between revisions
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*The general protocol for film preparation described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/08/29|2012/08/29]] was followed. The necessary amount of clay was added in the correct ratio. All films were prepared on a 0.5g scale. The films were placed in a freezer at -20°C immediately after pouring. These films will undergo the cyclic freeze-thaw procedure used for hydrogel preparation. | *The general protocol for film preparation described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/08/29|2012/08/29]] was followed. The necessary amount of clay was added in the correct ratio. All films were prepared on a 0.5g scale. The films were placed in a freezer at -20°C immediately after pouring. These films will undergo the cyclic freeze-thaw procedure used for hydrogel preparation. | ||
<br> | <br> | ||
Table | Table 2. Film Preparation | ||
<br> | <br> | ||
{| {{table}} | {| {{table}} | ||
| align="center" style="background:#f0f0f0;"|'''PVOH vs. Clay Ratio''' | | align="center" style="background:#f0f0f0;"|'''PVOH vs. Clay Ratio''' | ||
| align="center" style="background:#f0f0f0;"|'''Clay Selection''' | | align="center" style="background:#f0f0f0;"|'''Clay Selection''' | ||
| align="center" style="background:#f0f0f0;"|'''PVOH | | align="center" style="background:#f0f0f0;"|'''PVOH 130K Mass (g)''' | ||
| align="center" style="background:#f0f0f0;"|'''Actual Clay Mass (g)''' | | align="center" style="background:#f0f0f0;"|'''Actual Clay Mass (g)''' | ||
| align="center" style="background:#f0f0f0;"|'''H<sub>2</sub>O Added (mL)''' | | align="center" style="background:#f0f0f0;"|'''H<sub>2</sub>O Added (mL)''' | ||
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| 50:50||110% CEC Laponite w/ DMHXLBR||0.39820||0.10840||8.0 | | 50:50||110% CEC Laponite w/ DMHXLBR||0.39820||0.10840||8.0 | ||
|} | |} | ||
<br> | |||
==X-Ray Analysis== | |||
General Protocol: | |||
# Use a Kimwipe and acetone to thoroughly clean the low background sample holder | |||
# 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 | |||
# Turn on the chiller | |||
# Turn on Miniflex II. This is the white button on the machine | |||
# Turn on X-ray. The machine will be on when the red lights on the button labeled x-ray light up | |||
# Using a Geiger counter, test the radiation from the machine | |||
# Set sample in sample holder and record sample holder number | |||
# Close the door to the x-ray | |||
# Open software on computer | |||
*50:50 PVA 130K:110%LP was run on the x-ray. The data will be collected during the next session. | |||
==Hydrogel DSC preparation== | |||
*3mL of deionized H<sub>2</sub>O was added to each of the hydrogel samples. H<sub>2</sub>O was added in order to soften the hydrogels to allow DSC sample preparation. H<sub>2</sub>O was also added in order to remove any excess Rhodamine 6G still present. | |||
*The hydrogels will soak in deionized H<sub>2</sub>O until the next session. The water will be changed each day in order to remove the most Rhodamine 6G. | |||
==Microscope== | |||
* In order to determine if true microspheres had been prepared, it was necessary to view the prepared microspheres under a microscope. | |||
* To obtain true microspheres, the prepared samples were sonicated with a high power-probe sonicator. | |||
<br> | |||
General Protocol: | |||
# Remove microsphere samples from vial. Place microsphere samples in a clean, 50mL falcon tube. | |||
# Add 10mL deionized H<sub>2</sub>O to the tube. | |||
# Sonicate the microspheres using the high power probe sonicator for 3 minutes. | |||
'''Note''': Use protective ear equiptment whenever opearting the high power sonicator | |||
# Once the microspheres are completely mixed(the solution should be a milk white color), add a small amount of sample onto a glass slide using a Pasteur pipette. | |||
# View microspheres starting on the lowest magnification setting. | |||
<br> | |||
* Two microsphere samples were viewed under the microscope: PVA MW130,000 and 50:50 PVA 130,000:110% LP | |||
* When viewed, both samples contained microspheres. | |||
==Notes== | |||
*A plain oil sample will need to be run on the x-ray as a reference. Because of the presence of safflower oil in the prepared microsphere samples, the oil peak will be determined using the control oil spectrum. | |||
Revision as of 07:13, 19 April 2013
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Objectives
DSC
# 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
Film Preparation
X-Ray AnalysisGeneral Protocol:
Hydrogel DSC preparation
Microscope
Note: Use protective ear equiptment whenever opearting the high power sonicator
Notes
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