User:Karlena L. Brown/Notebook/PVOH Research/2013/02/04: Difference between revisions
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== | ==OBJECTIVES== | ||
''' | '''ACCIDENTALLY PLACED THIS ENTRY ON THE FEBRUARY 4th; HOWEVER, THIS ENTRY SHOULD BE UNDER FEBRUARY 6th. THANK YOU.''' | ||
* Begin preparing polyvinyl alcohol microsperes for experimental analysis | |||
* Filter surfactant exchanged modified clays | |||
* | * Complete freeze and thaw crosslinked clay cycle #1 | ||
* | |||
* | |||
''' | ==90:10 PVOH Clay Microsphere Preparations== | ||
'''*Reaction should be carried out using a reflux condenser and a thermostatic water bath of 55°C.''' | |||
# Dissolve ~ 1.0g total of PVOH 146K and clay additive selected (laponite) in 5mL hot deionized H<sub>2</sub>O | |||
# Acidify the solution using 0.25mL 0.5M H<sub>2</sub>SO<sub>4</sub> | |||
# Dissolve ~ 0.6g cellulose acetate butyrate (CAB) in 25mL 1,2-dichloroethane within a round bottom flask | |||
# Pour the acidified PVOH 146K solution into the 25mL 1,2-dichloroethane solution within the clean round bottom flask | |||
# Stir 1,2-dichloroethane, CAB, and PVOH 146K solution for 30 minutes | |||
# After 30 minutes of stirring, add 0.75mL glutaraldehyde to the solution | |||
# 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 | |||
# Wash the collected microspheres using ~ 2-3mL of the following solvents in the following order: | |||
'''* 1,2-dichloroethane''' | |||
'''* acetone''' | |||
'''* hot water''' | |||
'''* cold water''' | |||
'''* methanol''' | |||
# Scrape off all of the collected microspheres into a small glass vial. Leave the lid off of the small glass 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]''' | |||
<br> | |||
''' | {| {{table}} | ||
| align="center" style="background:#f0f0f0;"|'''Preparation of Laponite Microspheres using PVOH MW 146,000-186,000''' | |||
* | | align="center" style="background:#f0f0f0;"|'''''' | ||
* While | |- | ||
| PVOH 146K added(g)||0.9001 | |||
|- | |||
| Laponite clay added (g)||0.1004 | |||
|- | |||
| Cellulose Acetate Butyrate added (g)||0.6066 | |||
|- | |||
| Glutaraldehyde added (mL)||0.75 | |||
|- | |||
| H<sub>2</sub>SO<sub>4</sub> added (mL)||0.25 | |||
|} | |||
<br> | |||
==Important 1,2 Dichloroethane and Glutaraldehyde Safety== | |||
* Glutaldehyde is toxic colorless liquid '''(MW: 100.12 g / mole)''' | |||
* 1,2 Dichloroethane is a toxic colorless flammable liquid '''(MW: 98.96 g / mole)''' | |||
* Avoid all glutaldehyde and 1,2 dichloroethane skin contact by wearing gloves and googles | |||
* Glutaldehyde should be kept in the freezer when not in use | |||
* 1,2 Dichloroethane should be kept in a flammable cabinet when not in use | |||
* When in use, both glutaldehyde and 1,2 dichloroethane should be kept in the fume hood | |||
* 1,2 Dichloroethane should be capped at all times when not in use to inhibit inhalation and free floating volatile particles in the air | |||
* Keep the glutaldehyde vial in a beaker so that it does not spill | |||
* Keep anything and everything containing some form of 1,2 dichloroethane in the hood and allow all residue to evaporate off before washing | |||
* If spilled, wipe up glutaldehyde with paper towel while wearing gloves | |||
* If spilled, use a spill kit towel to soak up excess 1,2 dichloroethane. Allow some of the residual essence of 1,2 dichloroethane to evaporate; then use acetone to wipe over area contaminated with 1,2 dichloroethane. | |||
* Keep all spills of glutaldehyde and 1,2 dichloroethane contained in the fume hood | |||
* Wash hands after removing gloves that were in contact with glutaldehyde or 1,2 dichloroethane | |||
==Clay Exchanged Solutions & Vacuum Filtration Procedures== | |||
'''The clays being filtered are the clays that were prepared on 2/1/13''' | |||
'''Setup of a vacuum filtration system:''' | |||
* Clean 250mL Erlenmeyer Filter Flask | |||
* Large Buchner Funnel | |||
* Whatman #42 Filter Paper | |||
* Long Secure Rubber Hose | |||
# Filter a clay solution selected using the vacuum filtration system setup | |||
# Attach all parts of the apparatus to the vacuum filtrator system | |||
# Place a piece of Whatman #42 filter paper in the Buchner Funnel | |||
# Turn on the vacuum filtrator system | |||
# Check the suction rate to ensure that enough pressure is applied | |||
# Pour an exchanged clay solution into the Buchner funnel | |||
# Allow vacuum filtration to continue until the clay is completely dry | |||
# Discard the aqueous filtrate solution and place it in a labeled waste container | |||
# Collect the soil filtrate on the filter paper and scrape it into a small labeled metal pan | |||
# Place metal pan with the soil filtrate in the oven to dry for ~ 2-3 days | |||
# Wash all glassware and equipment first with H<sub>2</sub>O and then with acetone for later use | |||
==Notes== | |||
'''ACCIDENTALLY PLACED THIS ENTRY ON THE FEBRUARY 4th; HOWEVER, THIS ENTRY SHOULD BE UNDER FEBRUARY 6th. THANK YOU.''' | |||
* Clays previously prepared on 2/1/13 only exchanged for ~ 5 days rather than a week. | |||
* While attempting to filter the clays, due to vacuum filtration moving rather slowly during separation, clays only were filter for ~ 2.5 hours before actually being placed in the oven. | |||
* The temperature of the oven when the clays were placed in was ~ 90°C. | |||
* When removing clays from freeze and thaw process in cycle #1, many clays appeared to maintain ice crystals within their structure. | |||
* NaMT clays after freezing and thawing cycles appeared more rigid than laponite samples, but all in all PVOH 146K structure was maintained. | |||
* As freezing and thawing continued, PVOH 146K control sample became more crystalline and clear in appearance. | |||
* For all hydrogels that were removed with dye previous placed and attached within their contents, ~ 3mL of water was added to each beaker to analyze as well as quantify if and how much dye would leak out of each hydrogel. | |||
Revision as of 22:45, 10 February 2013
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OBJECTIVESACCIDENTALLY PLACED THIS ENTRY ON THE FEBRUARY 4th; HOWEVER, THIS ENTRY SHOULD BE UNDER FEBRUARY 6th. THANK YOU.
90:10 PVOH Clay Microsphere Preparations*Reaction should be carried out using a reflux condenser and a thermostatic water bath of 55°C.
* 1,2-dichloroethane * acetone * hot water * cold water * methanol
* The following procedure was adapted from the article Poly(vinyl alcohol) microspheres with pH- and thermosensitive properties as temperature-controlled drug delivery [1]
Important 1,2 Dichloroethane and Glutaraldehyde Safety
Clay Exchanged Solutions & Vacuum Filtration ProceduresThe clays being filtered are the clays that were prepared on 2/1/13 Setup of a vacuum filtration system: * Clean 250mL Erlenmeyer Filter Flask * Large Buchner Funnel * Whatman #42 Filter Paper * Long Secure Rubber Hose
NotesACCIDENTALLY PLACED THIS ENTRY ON THE FEBRUARY 4th; HOWEVER, THIS ENTRY SHOULD BE UNDER FEBRUARY 6th. THANK YOU.
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