User:Moira M. Esson/Notebook/CHEM-581/2012/10/26: Difference between revisions
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# Crosslink porphyrin films | # Crosslink porphyrin films | ||
# Run AA using film adsorption | # Run AA using film adsorption | ||
# Prepare next highest porphyrin concentration solution. Then add salts to these higher porphyrin solutions | # Prepare next highest porphyrin concentration solution. Then add salts to these higher porphyrin solutions | ||
<br> | |||
==Crosslinking== | |||
*The general protocol for porphyrin film crosslinking described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/14|2012/09/14]] was followed for the films listed below | |||
<br> | |||
'''Films Crosslinked''': | |||
#PVOH(22K) 1.0073g+1.0mL GA+1mL porphyrin | |||
#PVOH(22K) 1.05225g+1.0mL GA+1mL porphyrin | |||
<br> | |||
'''Crosslinking information''' | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Films''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount of fixant solution used to crosslink(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount fixant solution kept in vial(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount of 1% aqueous HCl solution used to crosslink(mL''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount HCl solution saved in vial(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount of 0.2M sodium bicarbonate used(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount sodium bicarbonate solution saved(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Mass of film after crosslinking(g)''' | |||
|- | |||
| PVOH(22K) 1.0073g+1.0mL GA+1mL porphyrin||99.95||13||100||14||100||12||1.4974 | |||
|- | |||
| PVOH(22K) 1.05225g+1.0mL GA+1mL porphyrin||101||12||98||13||99.8||12||1.9251 | |||
|} | |||
*For the films listed below, the films were placed in a 6M NaCl solution at 70°C for ~1.5 hours | |||
'''Crosslinked Films''': | |||
#PVOH(22K) 1.02114g+0.5mL GA+1mL porphyrin+HCl | |||
#PVOH(22K) 1.0067g+1mL GA+1mL porphyrin+HCl | |||
<br> | |||
'''Crosslinking information''': | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Films crosslinked''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount of NaCl added(g)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount 6M NaCl solution used(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Amount NaCl solution saved(mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Mass of film after crosslinking(g)''' | |||
|- | |||
| PVOH(22K) 1.02114g+0.5mL GA+1mL porphyrin+HCl||0.3576||100||12||1.7781 | |||
|- | |||
| PVOH(22K) 1.0067g+1mL GA+1mL porphyrin+HCl||0.363||99||12||1.5672 | |||
|} | |||
==Observations for crosslinking films== | |||
*PVOH(22K) 1.02114g+0.5mL GA+1mL porphyrin+HCl was shrunken, shriveled and was green in color before crosslinking | |||
*PVOH(22K) 1.0067g+1mL GA+1mL porphyrin+HCl shrunk, looked shriveled and was green in color before crosslinking | |||
*PVOH(22K) 1.0073g+1.0mL GA+1mL porphyrin was flat, relatively shiny and pink in color before crosslinking | |||
*PVOH(22K) 1.05225g+1.0mL GA+1mL porphyrin was flat, shiny and pink in color before crosslinking | |||
*When added film to fixant solution both beakers of solution had some color leak out. Color of both beakers were yellowish/greenish. Film with 1mL GA not as colored. Film with 0.5mL GA seems to be a more vibrant color(leaking more) | |||
*NaCl solution with film with 0.5mL GA had very slight leaking(slight discoloration of solution very light green). Coloration of solution was occurring very gradually | |||
*Both films after fixant solution were a vibrant green color(like jolly rancher green). Film with 1.0mL GA was a darker/ more vibrant green | |||
*Films placed in 1% aqueous HCl soltn. both started to have color leak out | |||
*1.0mL GA+HCl film when placed in the 6M NaCl solution leaked very minimally(solution looks very faintly green). Much less in comparison to 0.5mL GA. | |||
*0.5mL GA+HCl film after 1hr. and 15min. heated , remained bright green color. Stored in H<sub>2</sub>O. After adding H<sub>2</sub>O, film turned into a pink color(darker pink on edges) | |||
*Addition of both films to sodium bicarbonate caused all porphyrin to leak out(films no longer colored. completely clear.) | |||
*Film 1mLGA+HCl remained dark green and more stiff than other film. Turned pink after addition to deionized H<sub>2</sub>O | |||
<br> | |||
Please refer to [[User:Karlena_L._Brown/Notebook/CHEM-581/2012/10/26]] and [[User:Melissa_Novy/Notebook/CHEM-581/2012/10/26]] for calculations relating to preparation of higher concentration of porphyrin solutions and salt. | |||
==AA== | |||
*Ran AA following the general protocol for atomic absorption. Ran on solutions collected from film adsorption completed [[User:Moira_M._Esson/Notebook/CHEM-581/2012/10/17|2012/10/17]] | |||
<br> | |||
*Atomic Absorption Data | |||
{| {{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-CuSO<sub>4</sub>||7.4||0.37690||0.00430||5.63990 | |||
|- | |||
| ||10||0.47600||0.00620||7.01910 | |||
|- | |||
| 5 min NaMT-CuSO<sub>4</sub>||7.4||0.38080||0.00350||5.69420 | |||
|- | |||
| ||10||0.48150||0.00600||7.09560 | |||
|- | |||
| 10 min NaMT-CuSO<sub>4</sub>||7.4||0.29540||0.00370||4.50580 | |||
|- | |||
| ||10||0.37640||0.00480||5.63300 | |||
|- | |||
| 1 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.48030||0.00680||7.07890 | |||
|- | |||
| ||10||0.61880||0.00950||9.00630 | |||
|- | |||
| 5 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46120||0.00640||6.81310 | |||
|- | |||
| ||10||0.62080||0.00790||9.03420 | |||
|- | |||
| 10 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.43300||0.00400||6.42070 | |||
|- | |||
| ||10||0.62960||0.00480||9.15660 | |||
|- | |||
| 1 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.47470||0.00530||7.00100 | |||
|- | |||
| ||10||0.62050||0.00490||9.03000 | |||
|- | |||
| 5 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46110||0.00310||6.81170 | |||
|- | |||
| ||10||0.60940||0.00580||8.87550 | |||
|- | |||
| 10 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46800||0.00390||6.90770 | |||
|- | |||
| ||10||0.59620||0.00440||8.69180 | |||
|} | |||
<br> | |||
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Revision as of 12:22, 30 November 2012
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Objectives
Crosslinking
Crosslinked Films:
Observations for crosslinking films
AA
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