User:Moira M. Esson/Notebook/CHEM-581/2012/10/19: Difference between revisions
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#Finish running AA | #Finish running AA | ||
#Crosslink porphyrin films | #Crosslink porphyrin films | ||
#Reprepare Fe<sub>3</sub>O<sub>4</sub> filtrate that was prepared | #Reprepare Fe<sub>3</sub>O<sub>4</sub> filtrate that was prepared [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/26|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''': | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''''' | |||
| align="center" style="background:#f0f0f0;"|'''Concentration [ppm]''' | |||
| align="center" style="background:#f0f0f0;"|'''Abs. [ ]''' | |||
| align="center" style="background:#f0f0f0;"|'''BG''' | |||
| align="center" style="background:#f0f0f0;"|'''''' | |||
|- | |||
| ||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 | |||
|} | |||
<br> | |||
Using the following concentrations(shown above), a calibration curve was prepared. | |||
<br> | |||
[[Image:Cu%2B2_AAS_Calibration_Curve.png]] | |||
==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. | |||
*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
AA
AA Data collected:
Crosslinking
Crosslinking notes:
Fe3O4 Filtrates
Fe3O4 filtrate data
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