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

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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

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

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

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

ISE 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.

Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm)
8:50A 30 30 864
9:00A 30 30 869
9:30A 30 30 874
10:00A 30 30 865
10:30A 30 30 863
11:00A 30 29.5 861
11:30A 29.5 30 858
12:00P 30 30 853
3:15P 30 29.8 840
9:00P 29.8 28 819

ISE 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.

Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm)
8:50A 28 28 19.93
9:00A 28 29 23.13
9:30A 29 29 24.60
10:00A 29 28.5 27.20
10:30A 28.5 29 30.5
11:00A 29 29 33
11:30A 29 29 35.7
12:00P 29 29 38.9
3:15P 29 28.6 52.7
9:00P 28.6 27.2 76.2

Notes

  • 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).


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