User:Moira M. Esson/Notebook/CHEM-581/2012/10/19

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(Crosslinking)
Current revision (22:48, 10 November 2012) (view source)
(AA)
 
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Using the following concentrations(shown above), a calibration curve was prepared.
 +
<br>
 +
[[Image:Cu%2B2_AAS_Calibration_Curve.png]]
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==Crosslinking==
==Crosslinking==
*The general protocol for crosslinking glutaraldehyde films described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/14|2012/09/14]] was followed.  
*The general protocol for crosslinking glutaraldehyde films described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/14|2012/09/14]] was followed.  
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'''Crosslinking notes''':
'''Crosslinking notes''':
-
*While porphyrin film was in the H<sub>2</sub>SO<sub>4</sub> fixant solution, the film changed color from pink to yellow. Some yellow color leaked into the solution(uniformly). A good portion of color leaked out of
+
*While porphyrin film was in the H<sub>2</sub>SO<sub>4</sub> fixant solution, the film changed color from pink to yellow. Some yellow color leaked into the solution(uniformly). A good portion of color leaked out of during this step.
 +
*While taking out the film from the 1% aqueous HCl solution, the film did not have a frosted color to it(as other films not containing porphyrin had at this step). Instead, the film turned from yellowish to a relatively greenish tint. A good portion of color leaked out of the film during this step
 +
*When adding the film to the sodium bicarbonate solution, the film turned back into a light pinkish color. Color continued to leak out of film during this step. After 15 minutes the film still retained a faint pink color
 +
*From the amount of leakage, it appears as if 0.5mL glutaraldehyde per 1g PVOH in a large Teflon dish is not sufficient. For next film preparation, 1mL of glutaraldehyde will be used
 +
*approximately 12mL of each solution was saved after crosslinking
 +
==Fe<sub>3</sub>O<sub>4</sub> Filtrates==
 +
*It was observed that the Fe<sub>3</sub>O<sub>4</sub> filtrates all contained clay at the bottom of vial
 +
*The general protocol for adsorption of clays described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/26|2012/09/26]] in CuSO<sub>4</sub> was used
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'''Fe<sub>3</sub>O<sub>4</sub> filtrate data'''
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Amount clay used(g)'''
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| align="center" style="background:#f0f0f0;"|'''Time clay spun(min)'''
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|-
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| 0.1105||1
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|-
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| 0.1318||5
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|-
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| 0.1072||10
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|}
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*The filtrates appear to be more clear than when previously collected
 +
 

Current revision

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Objectives

  1. Finish running AA
  2. Crosslink porphyrin films
  3. Reprepare Fe3O4 filtrate that was prepared 2012/09/26

AA

  • Standard solutions were reprepared by Melissa Novy. Please refer to Melissa Novy's lab notebook for calculations and preparation

AA Data collected:

' Concentration [ppm] Abs. [ ] BG '
0.01-0.006000.00200
0.05-0.011600.00540
1-0.009200.00150
20.117100.00470
30.203300.00330
Given Conc. [ppm]Abs. [ ]BGConc. [ppm]
1 min NaMT-CuSO47.40.376900.004305.63990
100.476000.006207.01910
5 min NaMT-CuSO47.40.380800.003505.69420
100.481500.006007.09560
10 min NaMT-CuSO47.40.295400.003704.50580
100.376400.004805.63300
1 min 100%CEC NaMT-CuSO47.40.480300.006807.07890
100.618800.009509.00630
5 min 100%CEC NaMT-CuSO47.40.461200.006406.81310
100.620800.007909.03420
10 min 100%CEC NaMT-CuSO47.40.433000.004006.42070
100.629600.004809.15660
1 min 50%CEC NaMT-CuSO47.40.474700.005307.00100
100.620500.004909.03000
5 min 50%CEC NaMT-CuSO47.40.461100.003106.81170
100.609400.005808.87550
10 min 50%CEC NaMT-CuSO47.40.468000.003906.90770
100.596200.004408.69180


Using the following concentrations(shown above), a calibration curve was prepared.
Image:Cu+2_AAS_Calibration_Curve.png

Crosslinking

  • The general protocol for crosslinking glutaraldehyde films described on 2012/09/14 was followed.
  • For the films containing porphyrin, the exact amount of H2SO4 fixant solution used, 1% aqueous HCl solution used, and sodium bicarbonate solution used was recorded. Small samples of each of the three samples used for crosslinking were saved for later UV-vis analysis
' PVOH MW 22,000+ 0.5mL glutaraldehyde+ 1mL porphyrin PVOH MW 22,000+ 0.5mL glutaraldehyde+ NaMT PVOH MW 22,000+ 0.5mL glutaraldehyde+ 100%CEC
Amount solution 1 added(mL)100.0100.099.90
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)2.4394...3.0290

Crosslinking notes:

  • While porphyrin film was in the H2SO4 fixant solution, the film changed color from pink to yellow. Some yellow color leaked into the solution(uniformly). A good portion of color leaked out of during this step.
  • While taking out the film from the 1% aqueous HCl solution, the film did not have a frosted color to it(as other films not containing porphyrin had at this step). Instead, the film turned from yellowish to a relatively greenish tint. A good portion of color leaked out of the film during this step
  • When adding the film to the sodium bicarbonate solution, the film turned back into a light pinkish color. Color continued to leak out of film during this step. After 15 minutes the film still retained a faint pink color
  • From the amount of leakage, it appears as if 0.5mL glutaraldehyde per 1g PVOH in a large Teflon dish is not sufficient. For next film preparation, 1mL of glutaraldehyde will be used
  • approximately 12mL of each solution was saved after crosslinking

Fe3O4 Filtrates

  • It was observed that the Fe3O4 filtrates all contained clay at the bottom of vial
  • The general protocol for adsorption of clays described on 2012/09/26 in CuSO4 was used

Fe3O4 filtrate data

Amount clay used(g) Time clay spun(min)
0.11051
0.13185
0.107210
  • The filtrates appear to be more clear than when previously collected




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