User:Moira M. Esson/Notebook/CHEM-581/2013/02/06: Difference between revisions
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# Dissolve 1g total of PVA and clay additive in 5mL hot,deionized water. | # Dissolve 1g total of PVA and clay additive in 5mL hot,deionized water. | ||
# Acidify the solution using 0.25mL 0.5M H<sub>2</sub>SO<sub>4</sub>. | # Acidify the solution using 0.25mL 0.5M H<sub>2</sub>SO<sub>4</sub>. | ||
# Dissolve 0.6g Cellulose acetate butyrate in 25mL 1,2-dichloroethane. | # Dissolve 0.6g Cellulose acetate butyrate(CAB) in 25mL 1,2-dichloroethane. | ||
# Pour the acidified PVA solution into the 25mL 1,2-dichloroethane solution. | # Pour the acidified PVA solution into the 25mL 1,2-dichloroethane solution. Place all in a clean round bottom(RB) flask. | ||
# Stir the water/1,2-dichlorethane solution for 30 minutes. | # Stir the water/1,2-dichlorethane solution for 30 minutes. | ||
# After 30 minutes stirring, add 0.75mL glutaraldehyde to the solution. | # After 30 minutes stirring, add 0.75mL glutaraldehyde(GA) to the solution. | ||
# After the addition of glutaraldehyde, allow the reaction to carry out for 3 additional hours at 55°C. | # After the addition of glutaraldehyde, allow the reaction to carry out for 3 additional hours at 55°C. | ||
# Filter the produced microspheres from the solution using a a sintered glass filter and a vacuum. | # Filter the produced microspheres from the solution using a a sintered glass filter and a vacuum. | ||
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##cold water | ##cold water | ||
##methanol | ##methanol | ||
# | # Scrap all collected microspheres into a small vial. | ||
# Freeze microspheres in liquid nitrogen for ~2 minutes. | |||
# Place on [ask Dr. Hartings name of machine again] overnight to completely dry. | |||
*The following procedure was adapted from the article Poly(vinyl alcohol) microspheres with pH- and thermosensitive properties as temperature-controlled drug delivery [http://www.sciencedirect.com/science/article/pii/S1742706110002151] | *The following procedure was adapted from the article Poly(vinyl alcohol) microspheres with pH- and thermosensitive properties as temperature-controlled drug delivery [http://www.sciencedirect.com/science/article/pii/S1742706110002151] | ||
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| Amount of H2SO4 added(mL)||0.25 | | Amount of H2SO4 added(mL)||0.25 | ||
|} | |} | ||
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Observations: | Observations: | ||
*The dispersion agent(hereout referred to as CAB), lamponite clay and PVA formed a sort of suspension in the water/organic solvent solution. It did not appear to fully dissolve. Used a spatula to scrape the side of the RB flask in order to try and break up the large chunks. | *The dispersion agent(hereout referred to as CAB), lamponite clay and PVA formed a sort of suspension in the water/organic solvent solution. It did not appear to fully dissolve. Used a spatula to scrape the side of the RB flask in order to try and break up the large chunks. | ||
* After addition to heat, the large chunks generally broke apart. Small spheres seemed to be forming after approximately an hour spinning. | * After addition to heat, the large chunks generally broke apart. Small spheres seemed to be forming after approximately an hour spinning. | ||
*After 3 hour spinning and heat, large clumps of spheres formed. Upon scraping with a spatula these clumps broke apart into what appeared to be smaller spheres. | |||
*Large clumps indicates that we may want to change portion of our method to produce smaller microspheres. | |||
*The spheres were a cloudy, white color throughout. | |||
==Hydrogel Preparation== | ==Hydrogel Preparation== |
Revision as of 12:39, 6 February 2013
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Objectives
PVA MicrospheresGeneral Protocol:
Hydrogel Preparation
Clay Filtration |