User:Moira M. Esson/Notebook/CHEM-581/2012/10/26: Difference between revisions

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# 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
# Run UV-vis on film adsorption and porphyrin-salt solutions
<br>
<br>
==Crosslinking==
==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
*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
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| align="center" style="background:#f0f0f0;"|'''Films'''
| 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 of fixant solution used to crosslink(mL)'''
| align="center" style="background:#f0f0f0;"|''''''
| align="center" style="background:#f0f0f0;"|''''''
| align="center" style="background:#f0f0f0;"|''''''
| align="center" style="background:#f0f0f0;"|'''Amount fixant solution kept in vial(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 of 1% aqueous HCl solution used to crosslink(mL'''
Line 31: Line 28:
| align="center" style="background:#f0f0f0;"|'''Amount of 0.2M sodium bicarbonate used(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;"|'''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
| 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
| 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
*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

  1. Crosslink porphyrin films
  2. Run AA using film adsorption
  3. Prepare next highest porphyrin concentration solution. Then add salts to these higher porphyrin solutions


Crosslinking

  • The general protocol for porphyrin film crosslinking described on 2012/09/14 was followed for the films listed below


Films Crosslinked:

  1. PVOH(22K) 1.0073g+1.0mL GA+1mL porphyrin
  2. PVOH(22K) 1.05225g+1.0mL GA+1mL porphyrin


Crosslinking information

Films Amount of fixant solution used to crosslink(mL) Amount fixant solution kept in vial(mL) Amount of 1% aqueous HCl solution used to crosslink(mL Amount HCl solution saved in vial(mL) Amount of 0.2M sodium bicarbonate used(mL) Amount sodium bicarbonate solution saved(mL) 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:

  1. PVOH(22K) 1.02114g+0.5mL GA+1mL porphyrin+HCl
  2. PVOH(22K) 1.0067g+1mL GA+1mL porphyrin+HCl


Crosslinking information:

Films crosslinked Amount of NaCl added(g) Amount 6M NaCl solution used(mL) Amount NaCl solution saved(mL) 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 H2O. After adding H2O, 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 H2O


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 2012/10/17


  • Atomic Absorption Data
' 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




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