User:Madeleine Y. Bee/Notebook/CHEM-582 Experimental Chemistry II/2015/02/13

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February 13, 2015

  • Upscale syntheses of PVA-Alg-NaMT
  • Attempt regular synthesis with PVA-Alg-NaMT & AC to attempt to integrate AC into the nanocomposite structure

Procedure

Procedure adapted from | Kuo-Ying Amanda Wu and Keith D. Wisecarver (1992)

Upscaled 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)
    • 4 g of PVA and 0.64 g of sodium alginate in 7 mL of water (12.5% PVA and ~0.02% alginate)
      • Add alginate while stirring PVA-water solution
    • ~0.4 g NaMT should be added to this mixture where applicable
  2. Cool dissolved and mixed solution to 35°C
  3. Prepare 840 mL of saturated citric acid with 4% calcium chloride
    1. Add 33.6 g (4%) calcium chloride to 210 mL of water
    2. Add citric acid to saturation (48 g citric acid)
      • 14.7g/100mL > 30.87 g/210 for solubility comparable to boric acid
  4. 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
  5. Stir for 2 hrs to allow solidification
  6. Rinse with water to remove excess reactants


PVA-Alg-NaMT&AC

  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 and ~0.05 g AC should be added to this mixture where applicable
  2. Cool dissolved and mixed solution to 35°C
  3. Prepare 210 mL of saturated citric acid with 4% calcium chloride
    1. Add 8.4 g (4%) calcium chloride to 210 mL of water
    2. Add citric acid to saturation (12-15 g citric acid)
      • 14.7g/100mL > 30.87 g/210 for solubility comparable to boric acid
  4. 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
  5. Stir for 2 hrs to allow solidification
  6. Rinse with water to remove excess reactants

Measurements

  • PVA-Alg-NaMT
    • PVA: 4.01 g
    • Alg: 0.65 g
    • NaMT: 0.4 g
    • Citric acid: 48.03 g
    • CaCl2: 33.6 g
  • PVA-Alg-NaMT&AC
    • PVA: 1.01 g
    • Alg: 0.16 g
    • NaMT: 0.1 g
    • AC: 0.05 g
    • Citric acid: 12.69 g
    • CaCl2: 8.34 g

Notes

  • Run normal-scale PVA-Alg-NaMT with no citric acid
  • Mass out upscaled product, solvent washing and FTIR, pXRD


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