User:Eleni N. Kalivas/Notebook/CHEM-571/2015/02/06: Difference between revisions
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|style="background-color: #EEE"|[[Image:owwnotebook_icon.png|128px]]<span style="font-size:22px;"> PVA-Alg Bead Synthesis</span> | |||
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==February 6, 2015== | |||
*MG absorption/rehydration trial | |||
*PVA-Alg-Hectorite | |||
===Procedure=== | |||
Procedure adapted from [http://onlinelibrary.wiley.com/doi/10.1002/bit.260390411/abstract | Kuo-Ying Amanda Wu and Keith D. Wisecarver (1992)]<br.> | |||
Modified from [http://openwetware.org/wiki/User:Madeleine_Y._Bee/Notebook/CHEM-582_Experimental_Chemistry_II/2015/01/28 1/28/2015] | |||
# Prepare an aqueous solution of 13% PVA and 0.02% sodium alginate at 60°C (Stir plate on 3rd setting: ~68°C) | |||
#* 1 gram of PVA and 0.16 g of sodium alginate in 7 mL of water (12.5% PVA and ~0.02% alginate) | |||
##* Add alginate '''while stirring''' PVA-water solution | |||
#* ~0.1 g of nanocomposite should be added to this mixture where applicable | |||
# Cool dissolved and mixed solution to 35°C | |||
# Prepare 210 mL of saturated citric acid with 4% calcium chloride | |||
## Add 8.4 grams (4%) of calcium chloride to 210 mL of water | |||
## Add citric acid to saturation (32 g citric acid) | |||
##* 14.7g/100mL > 30.87 g/210 for solubility comparable to boric acid | |||
# Add the PVA-Alg-Nanocomposite mixture drop-wise (by syringe) to the gently stirring (stir plate 3) citric acid-calcium chloride solution using a Pasteur pipette | |||
# Stir for 2 hrs to allow solidification | |||
# Rinse with water to remove excess reactants | |||
====Measurements==== | |||
*PVA-Alg-Hectorite | |||
**PVA: 1.003 g | |||
**Alg: 0.161 g | |||
**Hectorite: 0.105 g | |||
**Citric acid: 12.751 g | |||
**CaCl<sub>2</sub>: 8.414 g | |||
*PVA-Alg-NaMT vial: 706 mg | |||
*PVA-Alg-NaMT upscale synthesis: 1470 mg | |||
====Notes==== | |||
*Rehydration attempt done on shaker, started at 12:28pm | |||
**Beads on bottom of vial separate into individuals beads as they rehydrate | |||
*Try lessening/removing citric acid | |||
*Observation: beads that hold up seem to sink to the bottom where as the ones that fall apart float | |||
====List of Characterization Techniques==== | |||
*UV-vis absorption (equilibrium measurements) | |||
*DSC: wet >before and after dehydration (structure & cross-linking) | |||
*pXRD dry (structure & cross-linking) | |||
*FTIR/solvent washing (bonds) | |||
*Microscopy: dry and wet (swelling, bead size)? | |||
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Revision as of 10:25, 11 February 2015
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