User:Karlena L. Brown/Notebook/PVOH Research/2012/10/31

OBJECTIVES

• Frepare PVOH film with 5-hydroxymethylfurfural
• Run FTIR analysis on all films prepared throughout the semester
• Run ion diffusion experiment on PVOH film and analyze data using Ion Selective Electrode

Furfural Film Preparation

• In 10mL beaker, weigh out ~ 1.0 grams PVOH (MW 22K)

(PVOH 22K Actual Mass = 1.0029g)

• Then, using a graduated cylinder add ~ 5 mL H₂O to the beaker
• After adding and combining PVOH (MW 22K) in a small beaker with H₂O, add a stir bar and prepare to stir solution
• On hot plate, stir and heat beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves
• Once PVOH solids thoroughly dissolve in solution, take the solution and place it in the fume hood
• Allow the solution to cool then add ~ 0.3g of 5-hydroxymethylfurfural to the solution

(Furfural Actual Mass = 0.3192g)

• Then pour the solution into a Teflon dish to sit, cool, and dry in the fume hood for ~ 2 days

Films Examined using FTIR

RECALL FTIR PROCEDURAL PROTOCOL 9/17/12

LIST OF FILMS FOR FTIR:

Ion Diffusion & Ion Selective Electrode Film Procedures

1. Cut small piece of PVOH 22K film containing 1mL glutaldehyde exchanged in CuSO₄ for 10 min
2. Place small cut piece of PVOH 22K film in plastic double graduated cylinder apparatus
3. Close and seal plastic double graduated cylinder apparatus
4. Next, in one graduated cylinder column pour in ~ 20mL of HPLC Grade H₂O
5. Then, in other graduated cylinder column pour in ~20mL of the varied ion concentrated solution
6. Plug the electrodes into the SympHony meter and turn on the ion selective electrode instruments
7. Then press the arrows until ISE (ion selective electrode) and μS/cm (microsiemen per centimeter) appear on the screen
8. Remove the electrodes from the storage solutions
9. Rinse the electrodes with distilled H₂O and thoroughly dry both with KimWipes
10. Place each electrode directly into the graduated cylinder columns containing either the HPLC Grade H₂O or the varied ion solution for analysis (one electrode per graduated column)
11. Measure the total amount of solution available and present for each graduated cylinder column
12. Let each solution and electrode equilibrate for a set period of time (between 2-5 minutes) and then press measure on each instrument
13. Once the measurement is finalized, record the values observed for each solution

Ensure the hole separating the two graduated cylinder columns is completely shielded and covered by the PVOH 22K film

Ion Diffusion Film Analysis: Varied Ion Solution

A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO₄ solution was used for an Ion Selective Electrode Analysis.

Ion Diffusion Film Analysis: HPLC Grade H₂O Solution

A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO₄ solution was used for an Ion Selective Electrode Analysis.

Notes

• The varied ion concentrated solution contained the following ions: Chlorine (Cl^-), Bromine (Br^-), and Iodine (I^-).
• μS/cm (microsiemen per centimeter) is a conductivity unit of measurement that is the inverse of an Ohm (O).
• Experimental readings regarding the Ion Selective Electrode Analysis were taken every 30 minutes; however, for the first reading and recording only a 10 min interval surpassed before a reading was taken.
• The final two readings germane to the Ion Selective Electrode Analysis for the PVOH 22K film containing 1mL glutaldehyde that was exchanged for 10 min with CuSO₄ were taken by Dr. Fox.
• A small leak was detected in the film used after several hours had passed (9:00P).