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

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(Notes)
Current revision (23:49, 14 December 2012) (view source)
(Films Examined using FTIR)
 
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==OBJECTIVES==
==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 H<sub>2</sub>O to the beaker
 +
* After adding and combining PVOH (MW 22K) in a small beaker with H<sub>2</sub>O, 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==
==Films Examined using FTIR==
 +
'''RECALL FTIR PROCEDURAL PROTOCOL 9/17/12'''
 +
 +
'''LIST OF FILMS FOR FTIR:'''
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Films'''
 +
| align="center" style="background:#f0f0f0;"|'''New mass(g)'''
 +
|-
 +
| PVOH(22K) 1.0067g+1mL GA+1mL porphyrin crosslinked||1.7688
 +
|-
 +
| PVOH(22K)+0.5mL GA+0.104g NaMT crosslinked spun 10 min CuSO4 prepared 10/17/2012||0.9465
 +
|-
 +
| PVOH(22K)+0.5mLGA+0.99mL porphyrin(no color on film )crosslinked prepared 10/19/2012||1.8045
 +
|-
 +
| PVOH(22K)+1mL GA+100%CEC crosslinked prepared 10/4/2012||1.3662
 +
|-
 +
| PVOH(22K)+1mL GA+1mL porphyrin crosslinked prepared 10/24/2012||1.5477
 +
|-
 +
| PVOH(22K)+0.5mL GA+1mL porphyrin crosslinked prepared 10/24/2012 #2||1.9685
 +
|-
 +
| PVOH(22K)+0.5mLGA+1mL porphyrin prepared crosslinked 10/26/2012||2.1206
 +
|-
 +
| PVOH(22K)+0.8wt% GA+100%CEC crosslinked spun 10 min CuSO4 prepared 10/26/2012||1.24
 +
|-
 +
| PVOH(22K)+0.8wt% GA+50% CEC crosslinked spun 10 min CuSO4 prepared 10/17/2012||1.074
 +
|}
 +
<br>
 +
[[Image:FTIR.JPG]]
 +
 +
==Ion Diffusion & Ion Selective Electrode Film Procedures==
 +
# Cut small piece of PVOH 22K film containing 1mL glutaldehyde exchanged in CuSO<sub>4</sub> for 10 min
 +
# Place small cut piece of PVOH 22K film in plastic double graduated cylinder apparatus
 +
# Close and seal plastic double graduated cylinder apparatus
 +
# Next, in one graduated cylinder column pour in ~ 20mL of HPLC Grade H<sub>2</sub>O
 +
# Then, in other graduated cylinder column pour in ~20mL of the varied ion concentrated solution
 +
# Plug the electrodes into the SympHony meter and turn on the ion selective electrode instruments
 +
# Then press the arrows until ISE (ion selective electrode) and μS/cm (microsiemen per centimeter) appear on the screen
 +
# Remove the electrodes from the storage solutions
 +
# Rinse the electrodes with distilled H<sub>2</sub>O and thoroughly dry both with KimWipes
 +
# Place each electrode directly into the graduated cylinder columns containing either the HPLC Grade H<sub>2</sub>O or the varied ion solution for analysis (one electrode per graduated column)
 +
# Measure the total amount of solution available and present for each graduated cylinder column
 +
# Let each solution and electrode equilibrate for a set period of time (between 2-5 minutes) and then press measure on each instrument
 +
# 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 Selective Electrode Film Procedures==
+
==Ion Diffusion Film Analysis: Varied Ion Solution==
-
==ISE Film Analysis: Varied Ion Solution==
+
'''A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO<sub>4</sub> solution was used for an Ion Selective Electrode Analysis.'''
'''A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO<sub>4</sub> solution was used for an Ion Selective Electrode Analysis.'''
Line 40: Line 102:
|}
|}
-
==ISE Film Analysis: HPLC Grade H<sub>2</sub>O Solution==
+
==Ion Diffusion Film Analysis: HPLC Grade H<sub>2</sub>O Solution==
'''A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO<sub>4</sub> solution was used for an Ion Selective Electrode Analysis.'''
'''A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO<sub>4</sub> solution was used for an Ion Selective Electrode Analysis.'''
Line 71: Line 133:
==Notes==
==Notes==
 +
* The varied ion concentrated solution contained the following ions: Chlorine (Cl<sup>-</sup>), Bromine (Br<sup>-</sup>), and Iodine (I<sup>-</sup>).
 +
* 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.
* 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 CuSO<sub>4</sub> were taken by Dr. Fox.  
* 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 CuSO<sub>4</sub> were taken by Dr. Fox.  

Current revision

PVOH Research Main project page
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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

LIST OF FILMS FOR FTIR:

Films New mass(g)
PVOH(22K) 1.0067g+1mL GA+1mL porphyrin crosslinked1.7688
PVOH(22K)+0.5mL GA+0.104g NaMT crosslinked spun 10 min CuSO4 prepared 10/17/20120.9465
PVOH(22K)+0.5mLGA+0.99mL porphyrin(no color on film )crosslinked prepared 10/19/20121.8045
PVOH(22K)+1mL GA+100%CEC crosslinked prepared 10/4/20121.3662
PVOH(22K)+1mL GA+1mL porphyrin crosslinked prepared 10/24/20121.5477
PVOH(22K)+0.5mL GA+1mL porphyrin crosslinked prepared 10/24/2012 #21.9685
PVOH(22K)+0.5mLGA+1mL porphyrin prepared crosslinked 10/26/20122.1206
PVOH(22K)+0.8wt% GA+100%CEC crosslinked spun 10 min CuSO4 prepared 10/26/20121.24
PVOH(22K)+0.8wt% GA+50% CEC crosslinked spun 10 min CuSO4 prepared 10/17/20121.074


Image:FTIR.JPG

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.

Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm)
8:50A3030864
9:00A3030869
9:30A3030874
10:00A3030865
10:30A3030863
11:00A3029.5861
11:30A29.530858
12:00P3030853
3:15P3029.8840
9:00P29.828819

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.

Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm)
8:50A282819.93
9:00A282923.13
9:30A292924.60
10:00A2928.527.20
10:30A28.52930.5
11:00A292933
11:30A292935.7
12:00P292938.9
3:15P2928.652.7
9:00P28.627.276.2

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).


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