User:Moira M. Esson/Notebook/CHEM-581/2012/10/03

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Objectives

  1. Finish crosslinking all films prepared with glutaraldehyde
  2. Use the ion selective electrode to measure the CuSO4 solutions made on 9/28/2012 by Melissa Novy and Karlena Brown
  3. Crosslink PVOH MW 130,000 film with [HCl]

Crosslinking

  1. The general protocol for crosslinking glutaraldehyde films described on 9/14/2012 was used


Crosslinking Glutaraldehyde films

' PVOH MW 22,000+ 0.8wt% glutaraldehyde+0.1010g 100% CEC surfactant clay PVOH MW 22,000+ 0.8wt% glutaraldehyde+NaMT PVOH MW 22,000+ 0.8wt% glutaraldehyde+PDMS
Amount solution 1 added(mL)100.0100.0100.0
Amount of 1% aqueous HCl added (mL)100.0100.098.0
Amount of 0.2M sodium bicarbonate solution added(mL)100.0100.0100.0
Amount of Sodium Bicarbonate added to sodium bicarbonate solution(g)1.68981.68091.6804
Mass of film after crosslinking (g)0.5519...0
  • Observations/Notes for crosslinking glutaraldehyde films:
    • The film placed in deionized H2O on 10/01/2012 was completely dissolved
    • When the PVOH MW 22,000+0.8wt%glutaraldehyde+PDMS film was first put into solution 1, the film was much more flimsy than any other film. The texture was more like glue than a rubber consistency as the other films
    • Upon adding the PVOH MW 22,000+0.8wt%glutaraldehyde+PDMS film to the 1% HCl solution, the film completely dissolved
    • Reviewing notes, it was observed that too little glutaraldehyde was added to each of the above mentioned films(only 8.4μL instead of 1mL).
    • New glutaraldehyde films(1.PVOH MW 22,000, 2.PVOH MW 22,000+replacing 5% of PVOH with PDMS, 3.PVOH MW 22,000+ 100% CEC surfactant clay, 4. PVOH MW 22,000+NaMT) using 1mL glutaraldehyde will be prepared
    • Although the clay films did not contain enough glutaraldehyde, the films did not dissolve and were able to complete crosslinking


2.The general protocol for crosslinking of PVOH films described on was used for crosslinking PVOH MW 130,000+[HCl]

  • Observations/Notes:
    • Crosslinked PVOH MW 130,000 film was a brown color and appeared more glossy than before. Although there was a color change, the brown color was not as dark as the crosslinked PVOH MW 22,000 films

Ion Selective Electrode

General Protocol:

  • The information from the ion selective electrode will be used to create a titration curve
  1. Choose the correct electrode and plug the electrode into the SympHony meter.
  2. Turn the meter on.
  3. Press the up or down arrows toward the bottom of the machine to choose the desired settings(in this case, choose ISE and mV).
  4. Remove the electrode from its storage solution.
  5. Rinse the end of the electrode with distilled H2O
  6. Dry the end of the electrode with a kimwipe(do not use a paper towel!)
  7. Make sure not to set the electrode down
  8. Place the electrode directly into the solution to be analyzed.
  9. If the electrode does not fit into the container that the solution to be analyzed is held in, the solution may be transferred to another clean container and measured from that container
  10. Let the solution and electrode equilibrate for 2 minutes, then press measure.
  11. Once the measurement is finalized, record the value that appears on the screen.


The general protocol for ion selective electrode was used for the collection of the ion selective electrode measurements

  • Upon testing the pH of our standard solutions, it was observed that the pH was too low(~7.8).
  • To adjust the pH of the solution, 0.1mL of ionic strength adjuster (4M pH adjuster containing NaOH) was added to each of the 3mL solutions before testing.
  • The ionic strength pH adjuster adjusted the pH of the solutions to a new pH value between 8 and 10.
  • The solvent for the solutions was deionized H2O unless otherwise specified


ISE and pH measurements

Solution Tested pH of solution with adjustment ISE values with adjustment[mV]
15ppm CuSO49.45-151.1
10ppm CuSO49.43-211.7
5ppm CuSO49.47-207.9
2ppm CuSO49.48-207.5
1ppm CuSO49.52-215.5
7.4ppm Cu2+ 100%CEC 1min filtrate9.53-201.2
10ppm Cu2+ 100%CEC 1min filtrate8.47-174.1
7.4ppm Cu2+ 100%CEC 5min filtrate9.52-200.5
10ppm Cu2+ 100%CEC 5min filtrate8.45-172.5
10ppm Cu2+ 100%CEC 10min filtrate8.51-172.3
7.4ppm Cu2+ 100%CEC 10min filtrate9.53-199.0
7.4ppm Cu2+ unmodified Na-MT 1min8.37-128.2
10ppm Cu2+ unmodified Na-MT 1min8.45-142.1
7.4ppm Cu2+ unmodified Na-MT 5min8.47-112.7
10ppm Cu2+ unmodified Na-MT 5min8.50-99.2
7.4ppm Cu2+ unmodified Na-MT 10min8.44-138.0
10ppm Cu2+ unmodified Na-MT 10min8.44-134.5

Film preparation

The general protocol for preparing PVOH films with glutaraldehyde described in entry 2012/09/12 was followed

  • Prepared ~1g PVOH MW 22,000+1mL glutaraldehyde
  • Prepared ~1g PVOH MW 22,000+1mL glutaraldehyde+100% CEC surfactant clay
  • Prepared ~1g PVOH MW 22,000+1mL glutaraldehyde+NaMT
  • Prepared ~1g PVOH MW 22,000+50% CEC surfactant clay

General Notes

  • Crosslinked glutaraldehyde film stored in deionized water on entry 2012/10/01 had completely dissolved in the beaker. This indicates that the film was not completely crosslinked







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