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

< User:Karlena L. Brown‎ | Notebook‎ | PVOH Research‎ | 2012‎ | 10
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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.

## Atomic Absorption NaMT-CuSO4 Exchanged Filtrate Solutions

 ' 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

## 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) 1.0073 1.0 1.0 N N PVOH 22K GA & PP(g) 1.0067 1.0 1.0 Y Y PVOH 22K GA & PP(g) 1.0523 0.5 1.0 N N PVOH 22K GA & PP(g) 1.0211 0.5 1.0 Y Y

## 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).