User:Sarah Burkhard/Notebook/CHEM 481 Polymers/2016/09/09

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Complete tasklist

    • Finish crosslinking for Glyoxal film. See protocol here
    • Redo beads formation, using powder clay instead of clay solution
  1. MG calibration curve
    • Carefully examine the bottom of your bottle. Any solid particles present?
    • We will use UV/Vis spectroscopy to measure MG concentrations
    • The maximum absorption for any UV/Vis analysis should be 1
    • You need at least 5 concentrations (as evenly distributed as possible) to make a standard curve
  2. PVOH film characterization
    • Swelling characteristics are examined by mass before and after drying in an oven
    • Crystallinity is examined using XRD
    • Thermal transitions are examined using DSC
  3. PVOH film preparation
    • Repeat the preparation of film containing clay, but use 3 wt% solution to replace some of the water.

3 wt% solution instead of powder for the following protocol: 1 g PVOH + 0.1 g bentonite + 0.5 mL glutaraldehyde in 12 mL water

wt% = weight of solute/ weight of solvent*100

3 wt% = 3 g bentonite / 97 ml water

0.1 g * 97 ml/3 g bentonite = 3.23 ml bentonite solution, 12 - 3.23 ml water

concentrated HCl is ~ 37 percent . To get 30 ml 10 percent, we need to dilute it with water .

21. 9 ml water + 8.1 ml HCl

multiplied by 5 -- ~100 ml water , 40 ml acid


  • Polyvinyl alcohol PVOH = PVA
  • Clay: Bentonite or NaMT

Bead formation

Make PVOH - clay - HCl solution

  • use powder clay
  • multiply the following by 4 to yield ~4.5 g of beads:

1.0016g PVOH and 0.1114g clay in 12 mL of HCl


  • 30 mL of ethyl acetate + 500 uL of glutaraldehyde
  • Add your PVA-clay (approximately .5 g of PVA and .051-.055g NaMT) in a dropwise manner. Immediately start timing the reaction for 2 minutes when you do the first drop.
  • After 2 minutes, slowly add 7 mL of 0.2 M NaHCO3.
  • Once completed, transfer to a falcon tube and centrifuge for 1 minute at 3000 rpm, rotor 41.
  • When beads are separated from the organic phase, pipet out the organic phase and re-suspend the beads in distilled water.


Glyoxal film formed a gel in HCl, which means crosslinking was not as successful as desired. We will discard it.