User:Madeleine Y. Bee/Notebook/CHEM-582 Experimental Chemistry II/2015/03/25

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March 25, 2015

  • repeat synthesis using syringe pump
  • prep more XRD samples (two additional types of beads)
  • prep Malachite Green samples for UV-Vis measurements


Procedure 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

  1. 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
  2. Cool dissolved and mixed solution to 35°C
  3. Prepare 210 mL of citric acid, calcium chloride solution
    1. Add 12 g (5%) citric acid
    2. Add 8.4 g (4%) calcium chloride
    3. Heat solution to 40°C while stirring
  4. Add the PVA-Alg-Nanocomposite mixture to a 10 ml syringe, carefully removing all air before tightening on the syringe tip
  5. Place the loaded syringe on the syringe pump, positioning the needle tip over the edge of the prepared citric acid/calcium chloride solution
  6. Set the syringe pump and press "run." The PVA solution will be added drop-wise to the cross-linking reaction mixture.
  7. Allow solution to cool to room temp while stirring for another 20 min
  8. Stir in 24 g (10%) citric acid solution for 30 min
  9. Stir in 14.9 g (0.5 M) sodium sulfate solution for 10 min
  10. Rinse with water to remove excess reactants
  11. Allow beads to dry in teflon plate overnight
  12. 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


  • PVA: 1.01 g
  • Alg: 0.16 g
  • NaMT: 0.1 g
  • citric acid: 12.22 g
  • CaCl2: 8.40 g
  • citric acid: 11.98 + 12.24 g
  • sodium sulfate: 14.94 g


10 (9.5 actual) mL at 1.5 mL/m


  • Ground up beads for XRD