Objectives
- Finish running AA
- Crosslink porphyrin films
- Reprepare Fe3O4 filtrate that was prepared 2012/09/26
AA
- Standard solutions were reprepared by Melissa Novy. Please refer to Melissa Novy's lab notebook for calculations and preparation
AA Data collected:
| '
| 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
|
Using the following concentrations(shown above), a calibration curve was prepared.
Crosslinking
- The general protocol for crosslinking glutaraldehyde films described on 2012/09/14 was followed.
- For the films containing porphyrin, the exact amount of H2SO4 fixant solution used, 1% aqueous HCl solution used, and sodium bicarbonate solution used was recorded. Small samples of each of the three samples used for crosslinking were saved for later UV-vis analysis
| '
| PVOH MW 22,000+ 0.5mL glutaraldehyde+ 1mL porphyrin
| PVOH MW 22,000+ 0.5mL glutaraldehyde+ NaMT
| PVOH MW 22,000+ 0.5mL glutaraldehyde+ 100%CEC
|
| Amount solution 1 added(mL) | 100.0 | 100.0 | 99.90
|
| Amount of 1% aqueous HCl added (mL) | 100.0 | 100.0 | 98.0
|
| Amount of 0.2M sodium bicarbonate solution added(mL) | 100.0 | 100.0 | 100.0
|
| Amount of Sodium Bicarbonate added to sodium bicarbonate solution(g) | 1.6898 | 1.6809 | 1.6804
|
| Mass of film after crosslinking (g) | 2.4394 | ... | 3.0290
|
Crosslinking notes:
- While porphyrin film was in the H2SO4 fixant solution, the film changed color from pink to yellow. Some yellow color leaked into the solution(uniformly). A good portion of color leaked out of during this step.
- While taking out the film from the 1% aqueous HCl solution, the film did not have a frosted color to it(as other films not containing porphyrin had at this step). Instead, the film turned from yellowish to a relatively greenish tint. A good portion of color leaked out of the film during this step
- When adding the film to the sodium bicarbonate solution, the film turned back into a light pinkish color. Color continued to leak out of film during this step. After 15 minutes the film still retained a faint pink color
- From the amount of leakage, it appears as if 0.5mL glutaraldehyde per 1g PVOH in a large Teflon dish is not sufficient. For next film preparation, 1mL of glutaraldehyde will be used
- approximately 12mL of each solution was saved after crosslinking
Fe3O4 Filtrates
- It was observed that the Fe3O4 filtrates all contained clay at the bottom of vial
- The general protocol for adsorption of clays described on 2012/09/26 in CuSO4 was used
Fe3O4 filtrate data
| Amount clay used(g)
| Time clay spun(min)
|
| 0.1105 | 1
|
| 0.1318 | 5
|
| 0.1072 | 10
|
- The filtrates appear to be more clear than when previously collected
|
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