User:Karlena L. Brown/Notebook/PVOH Research/2012/10/19

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OBJECTIVES

  • Prepare new CuSO4 standards for Atomic Absorption
  • Re-examine NaMT-CuSO4 exchanged filtrate solutions using Atomic Absorption
  • Crosslink all porphyrin films prepared
  • Prepare new crosslinking fixant solutions

New CuSO4 Dilution Standards for Atomic Absorption

  • Solution 0.1 ppm CuSO4
  (20 ppm CuSO4)V1 = (0.1 ppm CuSO4)(12mL)
   V1 = 0.6mL of 20 ppm CuSO4
  • Solution 0.5 ppm CuSO4 requires
  (20 ppm CuSO4)V1 = (0.5 ppm CuSO4)(12mL)
   V1 = 1.2mL of 20 ppm CuSO4
  • Solution 1 ppm CuSO4 requires
  (20 ppm CuSO4)V1 = (1 ppm CuSO4)(12mL)
   V1 = 3mL of 20 ppm CuSO4
  • Solution 2 ppm CuSO4 requires
  (20 ppm CuSO4)V1 = (2 ppm CuSO4)(12mL)
   V1 = 6mL of 20 ppm CuSO4
  • Solution 3 ppm CuSO4 requires
  (20 ppm CuSO4)V1 = (3 ppm CuSO4)(12mL)
   V1 = 9mL of 20 ppm CuSO4

Using the following concentrations(shown above), a calibration curve was prepared.
Image:Cu+2_AAS_Calibration_Curve.png

Atomic Absorption NaMT-CuSO4 Exchanged Filtrate Solutions

' Concentration [ppm] Abs. [ ] BG '
0.01-0.006000.00200
0.05-0.011600.00540
1-0.009200.00150
20.117100.00470
30.203300.00330
Given Conc. [ppm]Abs. [ ]BGConc. [ppm]
1 min NaMT-CuSO47.40.376900.004305.63990
100.476000.006207.01910
5 min NaMT-CuSO47.40.380800.003505.69420
100.481500.006007.09560
10 min NaMT-CuSO47.40.295400.003704.50580
100.376400.004805.63300
1 min 100%CEC NaMT-CuSO47.40.480300.006807.07890
100.618800.009509.00630
5 min 100%CEC NaMT-CuSO47.40.461200.006406.81310
100.620800.007909.03420
10 min 100%CEC NaMT-CuSO47.40.433000.004006.42070
100.629600.004809.15660
1 min 50%CEC NaMT-CuSO47.40.474700.005307.00100
100.620500.004909.03000
5 min 50%CEC NaMT-CuSO47.40.461100.003106.81170
100.609400.005808.87550
10 min 50%CEC NaMT-CuSO47.40.468000.003906.90770
100.596200.004408.69180


Fixant Solution Preparation

  1. Weigh out ~200g Na2SO4
 (Actual Na2SO4 Mass: 199.9953g)
  1. Add the Na2SO4 solids to a 1000mL closed cap plastic bottle
  2. Next, add ~1000mL of H2O to the bottle along with large magnetic stir bar
  3. Place container with the solution on a stir plate and stir solution for ~20 minutes or until all solids dissipate into solution
  4. Add 20mL of concentrated H2SO4 to solution and continue stirring for ~10 minutes more

Crosslinking Porphyrin Films

RECALL PROTOCOL REGARDING CROSSLINKING GLUTALDEHYDE FILMS 9/21/12; however, pay attention to the two PVOH films that will not be placed in the fixant solution during the crosslinking procedure.

Films Prepared PVOH 22K Amount (g) Glutaldehyde Amount (mL) Porphyrin Amount (mL) HCl Addition (Y/N) Fixant Solution (Y/N)
PVOH 22K GA & PP(g)1.00731.01.0NN
PVOH 22K GA & PP(g)1.00671.01.0YY
PVOH 22K GA & PP(g)1.05230.51.0NN
PVOH 22K GA & PP(g)1.02110.51.0YY

Notes

  • For PVOH 22K glutaldehyde porphyrin films that were crosslinked, all films maintained a swirled light pink / salmon color appearance.
  • During crosslinking and excessive heating, the porphyrin films began to turn lime green; most films turned green upon entering the fixant solution composed of Na2SO4 and H2SO</sub>4</sub>.
  • However, the PVOH films in which two drops of HCl were added, initially started and appeared green before crosslinking.
  • Most PVOH 22K glutaldehyde porphyrin films had some amount of porphyrin leach out into various solutions during crosslinking. Many solutions maintained a yellow green / mantis green appearance after the removal of porphyrin films.
  • For this reason, after every switch or movement of a porphyrin film to another solution, a small amount (10mL) of each solution was collected for UV-Vis analysis. After crosslinking, all films were then stored in beakers full of distilled H2O.
  • Upon entering the distilled H2O, each film reverted back and turned pink in color again (darker pink on edges).



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