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
(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
RECALL ATOMIC ABSORPTION PROCEDURAL PROTOCOL 10/02/12
Atomic Absorption Data and Calibration Curve Data from AA wizard:
'
|
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
- Weigh out ~200g Na2SO4
(Actual Na2SO4 Mass: 199.9953g)
- Add the Na2SO4 solids to a 1000mL closed cap plastic bottle
- Next, add ~1000mL of H2O to the bottle along with large magnetic stir bar
- Place container with the solution on a stir plate and stir solution for ~20 minutes or until all solids dissipate into solution
- 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 H2SO4.
- 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).
|