- 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:
||Abs. [ ]
| ||Given Conc. [ppm]||Abs. [ ]||BG||Conc. [ppm]
| 1 min NaMT-CuSO4||7.4||0.37690||0.00430||5.63990
| 5 min NaMT-CuSO4||7.4||0.38080||0.00350||5.69420
| 10 min NaMT-CuSO4||7.4||0.29540||0.00370||4.50580
| 1 min 100%CEC NaMT-CuSO4||7.4||0.48030||0.00680||7.07890
| 5 min 100%CEC NaMT-CuSO4||7.4||0.46120||0.00640||6.81310
| 10 min 100%CEC NaMT-CuSO4||7.4||0.43300||0.00400||6.42070
| 1 min 50%CEC NaMT-CuSO4||7.4||0.47470||0.00530||7.00100
| 5 min 50%CEC NaMT-CuSO4||7.4||0.46110||0.00310||6.81170
| 10 min 50%CEC NaMT-CuSO4||7.4||0.46800||0.00390||6.90770
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.
||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
- 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).