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

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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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