User:James C. Schwabacher/Notebook/CHEM-571/2015/03/20: Difference between revisions
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==March 20, 2015== | |||
*repeat synthesis using syringe pump | |||
*prep XRD samples (two types of beads) | |||
===Procedure=== | |||
Procedure adapted from [http://onlinelibrary.wiley.com/doi/10.1002/bit.260390411/abstract | Kuo-Ying Amanda Wu and Keith D. Wisecarver (1992)] and [http://www.sciencedirect.com/science/article/pii/S1369703X10000768 Hydrolysis of liquid pineapple waste by invertase immobilized in PVA–alginate matrix]<br.> | |||
<br.> | |||
PVA-Alg-NaMT | |||
# Prepare an aqueous solution of 13% PVA and 0.02% sodium alginate at 60°C (Stir plate on 3rd setting: ~68°C) | |||
#* '''1 g 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 NaMT''' should be added to this mixture where applicable | |||
# Cool dissolved and mixed solution to 35°C | |||
# Prepare 210 mL of citric acid, calcium chloride solution | |||
## Add '''12 g (5%) citric acid''' | |||
## Add '''8.4 g (4%) calcium chloride''' | |||
## Heat solution to 40°C while stirring | |||
# Add the PVA-Alg-Nanocomposite mixture to a 10 ml syringe, carefully removing all air before tightening on the syringe tip | |||
# Place the loaded syringe on the syringe pump, positioning the needle tip over the edge of the prepared citric acid/calcium chloride solution | |||
# Set the syringe pump and press "run." The PVA solution will be added drop-wise to the cross-linking reaction mixture. | |||
#Allow solution to cool to room temp while stirring for another 20 min | |||
# Stir in '''24 g''' (10%) citric acid solution for 30 min | |||
# Stir in '''14.9 g''' (0.5 M) sodium sulfate solution for 10 min | |||
# Rinse with water to remove excess reactants | |||
# Allow beads to dry in teflon plate overnight | |||
# Clean syringe | |||
#* Pass syringe tip over flame, solution will burst out | |||
#* Use syringe to push water through tip to get any remaining solution out | |||
#* Rinse again with water until solution runs clear | |||
====Measurements==== | |||
*PVA: 1.01 g | |||
*Alg: 0.16 g | |||
*NaMT: 0.1 g | |||
*citric acid: 12.0 g | |||
*CaCl2: 8.44 g | |||
*citric acid: 11.59 + 12.05 g | |||
*sodium sulfate: 14.94 g | |||
====Notes==== | |||
== | *Ground up beads for XRD | ||
== | |||
* | |||
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Revision as of 19:56, 1 April 2015
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March 20, 2015
ProcedureProcedure adapted from | Kuo-Ying Amanda Wu and Keith D. Wisecarver (1992) and Hydrolysis of liquid pineapple waste by invertase immobilized in PVA–alginate matrix<br.> <br.> PVA-Alg-NaMT
Measurements
Notes
|