Difference between revisions of "User:Moira M. Esson/Notebook/CHEM-581/2012/10/19"

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(Crosslinking)
(AA)
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| ||10||0.59620||0.00440||8.69180
 
| ||10||0.59620||0.00440||8.69180
 
|}
 
|}
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<br>
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Using the following concentrations(shown above), a calibration curve was prepared.
 +
<br>
 +
[[Image:Cu%2B2_AAS_Calibration_Curve.png]]
 +
 
==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.  
 
*For the films containing porphyrin, the exact amount of H<sub>2</sub>SO<sub>4</sub> 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
 
*For the films containing porphyrin, the exact amount of H<sub>2</sub>SO<sub>4</sub> 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
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|''''''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH MW 22,000+ 0.5mL glutaraldehyde+ 1mL porphyrin'''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH MW 22,000+ 0.5mL glutaraldehyde+ NaMT'''
 +
| align="center" style="background:#f0f0f0;"|'''PVOH MW 22,000+ 0.5mL glutaraldehyde+ 100%CEC'''
 +
|-
 +
| Amount solution 1 added(mL)||100.0||100.0||99.90
 +
|-
 +
| Amount of 1% aqueous HCl added (mL)||100.0||100.0||98.0
 +
|-
 +
| Amount of 0.2M sodium bicarbonate solution added(mL)||100.0||100.0||100.0
 +
|-
 +
| Amount of Sodium Bicarbonate added to sodium bicarbonate solution(g)||1.6898||1.6809||1.6804
 +
|-
 +
| Mass of film after crosslinking (g)||2.4394||...||3.0290
 +
|}
 +
'''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 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
 +
'''Fe<sub>3</sub>O<sub>4</sub> filtrate data'''
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Amount clay used(g)'''
 +
| align="center" style="background:#f0f0f0;"|'''Time clay spun(min)'''
 +
|-
 +
| 0.1105||1
 +
|-
 +
| 0.1318||5
 +
|-
 +
| 0.1072||10
 +
|}
 +
*The filtrates appear to be more clear than when previously collected
 +
 
  
  

Revision as of 19:48, 10 November 2012

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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 -0.00600 0.00200
0.05 -0.01160 0.00540
1 -0.00920 0.00150
2 0.11710 0.00470
3 0.20330 0.00330
Given Conc. [ppm] Abs. [ ] BG Conc. [ppm]
1 min NaMT-CuSO4 7.4 0.37690 0.00430 5.63990
10 0.47600 0.00620 7.01910
5 min NaMT-CuSO4 7.4 0.38080 0.00350 5.69420
10 0.48150 0.00600 7.09560
10 min NaMT-CuSO4 7.4 0.29540 0.00370 4.50580
10 0.37640 0.00480 5.63300
1 min 100%CEC NaMT-CuSO4 7.4 0.48030 0.00680 7.07890
10 0.61880 0.00950 9.00630
5 min 100%CEC NaMT-CuSO4 7.4 0.46120 0.00640 6.81310
10 0.62080 0.00790 9.03420
10 min 100%CEC NaMT-CuSO4 7.4 0.43300 0.00400 6.42070
10 0.62960 0.00480 9.15660
1 min 50%CEC NaMT-CuSO4 7.4 0.47470 0.00530 7.00100
10 0.62050 0.00490 9.03000
5 min 50%CEC NaMT-CuSO4 7.4 0.46110 0.00310 6.81170
10 0.60940 0.00580 8.87550
10 min 50%CEC NaMT-CuSO4 7.4 0.46800 0.00390 6.90770
10 0.59620 0.00440 8.69180


Using the following concentrations(shown above), a calibration curve was prepared.
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) 100.0 100.0 99.90
Amount of 1% aqueous HCl added (mL) 100.0 100.0 98.0
Amount of 0.2M sodium bicarbonate solution added(mL) 100.0 100.0 100.0
Amount of Sodium Bicarbonate added to sodium bicarbonate solution(g) 1.6898 1.6809 1.6804
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)
0.1105 1
0.1318 5
0.1072 10
  • The filtrates appear to be more clear than when previously collected