User:Rachel Gill/Notebook/Chem 681 2018/2018/11/09

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Objective

  • Make 10% Chitosan with 10% HCl to see if that can be used in place of PVA to hold montmorillonite. Learn how to used the SEM and take photos of PVA and PVA/clay beads.

Lab Protocol

  • Chitosan solution:
    • Tube 1: 5.03225 g chitosan, 45.01566 g 10% HCl
    • Tube 2: 4.96347 g chitosan, 45.19017 g 10% HCl

SEM How to

  1. Turn key to start
  2. Wait for Evac to stop blinking then click vent
  3. Open chamber
  4. Prepare samples by cutting carbon fiber tape and putting then on sample stand that has small circles on it.
  5. Slide sample stand on gold sample holder curve part faces back
  6. Evac, raise beam 10 mm (knob on top of sample chamber)
  7. turn on computer
  8. chamberscope - camber for inside
  9. in touch scope (without circle) open once evac stops blinking
  10. observe turns on beam, clicking on screen moves camera to that location
  11. WB on bottom left, set to 10 mm
  12. to pull up stage selecting click grey arrow in right most corner
  13. ACB when you first look at sample (auto contrast and brightness)
  14. change probe current, zoomed in low 30, zoomed out high 50
  15. zoom in as much as you want, click RDC to pull up small window to play with course and fine adjustment (bottom right, use mouse wheel to adjust)
  16. to save image: settings -> SEM -> user name image -> change count number to 1 for first sample
  17. click on camera icon to take picture
  18. click fast when done
  19. observe turn off beam, vent, and raise beam 20-30 mm
  20. when vent stops blinking take out sample, close chamber and press evac
  21. when evac stops blinking shut down software then turn key to 0 (off)

Data

PVA beads

PVA 1 0001.jpg

PVA 1 0002.jpg

PVA/clay beads

PVA clay 1 0003.jpg

PVA clay 1 0005.jpg

PVA clay 1 0001.jpg

PVA clay 1 0002.jpg

PVA clay 1 0006.jpg

New Samples of PVA beads DSC

  • sample 1: pan mass 40.44 mg, sample mass 3.83 mg
  • sample 2: pan mass 40.53 mg, sample mass 3.73 mg
  • reference pan: 40.12 mg

MG dye uptake for PVA beads

  • sample 1: beads 0.10146 g, 0.5 ppm MG 5.00681 g
  • sample 2: beads 0.10023 g, 1.00 ppm MG 5.00132 g
  • sample 3: beads 0.10032 g, 1.53 ppm MG 5.04375 g
  • sample 4: beads 0.10070 g, 3 ppm MG 5.02209 g
  • sample 5: beads 0.10068 g, 8.88 ppm MG 5.02565 g
  • sample 6: beads 0.10010 g, 15.3 ppm MG 5.01107 g
  • sample 7: beads 0.10009 g, 25.3 ppm MG 5.00905 g
  • sample 1A: beads 0.10007 g, 0.5 ppm MG 5.02098 g
  • sample 2A: beads 0.10089 g, 1.00 ppm MG 5.02039 g
  • sample 3A: beads 0.10088 g, 1.53 ppm MG 5.01322 g
  • sample 4A: beads 0.99983 g, 3 ppm MG 5.00572 g
  • sample 5A: beads 0.10095 g, 8.88 ppm MG 5.02091 g
  • sample 6A: beads 0.10050 g, 15.3 ppm MG 5.00876 g
  • sample 7A: beads 0.10083 g, 25.3 ppm MG 5.02333 g

Notes