User:Rachel Gill/Notebook/Chem 681 2018/2018/10/31

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Objective

To analyze particles using DSC (differential scanning calorimetry), hydration test, and image analysis to determine size of particles.

Lab Protocol

  • PVA/caly composite beads were generated using previous set up.
  • DSC samples were prepared by first weighting Tzero pans and then weighing out approximately 3-5 mg of sample that was to be analyzed.
  • Hydration test was done by adding approximately 100 mg of PVA/clay beads and PVA beads to a large falcon tube and then filling them with 50 g of distilled water. The mass of the beads would then be measured after a week had passed to see how much water they had adsorbed.

Data

DSC Analysis

  • PVA/clay beads
    • RL: Tzero pan mass 40.76 mg, sample mass 3.42 mg
    • JN: Tzero pan mass 40.79 mg, sample mass 4.52 mg
    • AJRL Tzero pan mass 40.92 mg, sample mass 3.22 mg
    • JB Tzero pan mass 40.62 mg, sample mass 3.44 mg
    • RG Tzero pan mass 40.47 mg, sample mass 3.02 mg
  • PVA (Sigma Aldrich), lot#MKBJ6397V, Mw 31,000-50,000, 98-99% hydrolyzed
    • RL:pan mass 40.74 mg, sample mass 4.50 mg
    • JN: pan mass 40.48 mg, sample mass 4.38 mg
    • AJRL: pan mass 40.57 mg, sample mass 5.41 mg
    • JB: pan mass 40.24 mg, sample mass 3.21 mg
    • RG: pan mass 40.59 mg, sample mass 4.74 mg

DSC Procedure

  • equil 20 degrees C
  • isothermal for 1 minute
  • ramp 10 degrees C/minute to 250 degrees C
  • isothermal for 1 minute
  • ramp 10 degrees C/minute to 20 degrees C
  • repeat segment 2 for 1 times

Hydration Test

  • PVA/clay beads
    • sample 1: 0.12511 g beads, 52.2327 g water
    • sample 2: 0.126141 g beads, 50.1840 g water
  • PVA beads
    • sample 1: 0.12639 g beads, 50.0187 g water
    • sample 2: 0.12515 g beads, 50.0760 g water

Notes

  • DSC was done to measure transitions, 1st melting crystalline to liquid, 2nd glass transition amorphous stuck in place to amorphous to wiggling.