User:Karlena L. Brown/Notebook/PVOH Research/2012/10/19: Difference between revisions
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V<sub>1</sub> = 9mL of 20 ppm CuSO<sub>4</sub> | V<sub>1</sub> = 9mL of 20 ppm CuSO<sub>4</sub> | ||
Using the following concentrations(shown above), a calibration curve was prepared. | '''Using the following concentrations(shown above), a calibration curve was prepared.''' | ||
<br> | <br> | ||
[[Image:Cu%2B2_AAS_Calibration_Curve.png]] | [[Image:Cu%2B2_AAS_Calibration_Curve.png]] | ||
==Atomic Absorption NaMT-CuSO4 | ==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:''' | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''''' | |||
| align="center" style="background:#f0f0f0;"|'''Concentration [ppm]''' | |||
| align="center" style="background:#f0f0f0;"|'''Abs. [ ]''' | |||
| align="center" style="background:#f0f0f0;"|'''BG''' | |||
| align="center" style="background:#f0f0f0;"|'''''' | |||
|- | |||
| ||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-CuSO<sub>4</sub>||7.4||0.37690||0.00430||5.63990 | |||
|- | |||
| ||10||0.47600||0.00620||7.01910 | |||
|- | |||
| 5 min NaMT-CuSO<sub>4</sub>||7.4||0.38080||0.00350||5.69420 | |||
|- | |||
| ||10||0.48150||0.00600||7.09560 | |||
|- | |||
| 10 min NaMT-CuSO<sub>4</sub>||7.4||0.29540||0.00370||4.50580 | |||
|- | |||
| ||10||0.37640||0.00480||5.63300 | |||
|- | |||
| 1 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.48030||0.00680||7.07890 | |||
|- | |||
| ||10||0.61880||0.00950||9.00630 | |||
|- | |||
| 5 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46120||0.00640||6.81310 | |||
|- | |||
| ||10||0.62080||0.00790||9.03420 | |||
|- | |||
| 10 min 100%CEC NaMT-CuSO<sub>4</sub>||7.4||0.43300||0.00400||6.42070 | |||
|- | |||
| ||10||0.62960||0.00480||9.15660 | |||
|- | |||
| 1 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.47470||0.00530||7.00100 | |||
|- | |||
| ||10||0.62050||0.00490||9.03000 | |||
|- | |||
| 5 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46110||0.00310||6.81170 | |||
|- | |||
| ||10||0.60940||0.00580||8.87550 | |||
|- | |||
| 10 min 50%CEC NaMT-CuSO<sub>4</sub>||7.4||0.46800||0.00390||6.90770 | |||
|- | |||
| ||10||0.59620||0.00440||8.69180 | |||
|} | |||
<br> | |||
==Fixant Solution Preparation== | ==Fixant Solution Preparation== | ||
# Weigh out ~200g Na<sub>2</sub>SO<sub>4</sub> | |||
'''(Actual Na<sub>2</sub>SO<sub>4</sub> Mass: 199.9953g)''' | |||
# Add the Na<sub>2</sub>SO<sub>4</sub> solids to a 1000mL closed cap plastic bottle | |||
# Next, add ~1000mL of H<sub>2</sub>O 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 H<sub>2</sub>SO<sub>4</sub> 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. | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Films Prepared''' | |||
| align="center" style="background:#f0f0f0;"|'''PVOH 22K Amount (g)''' | |||
| align="center" style="background:#f0f0f0;"|'''Glutaldehyde Amount (mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''Porphyrin Amount (mL)''' | |||
| align="center" style="background:#f0f0f0;"|'''HCl Addition (Y/N)''' | |||
| align="center" style="background:#f0f0f0;"|'''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 Na<sub>2<sub>SO</sub>4</sub> and H<sub>2</sub>SO</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 H<sub>2</sub>O. | |||
* Upon entering the distilled H<sub>2</sub>O, each film reverted back and turned pink in color again (darker pink on edges). | |||
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Revision as of 01:56, 24 November 2012
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OBJECTIVES
New CuSO4 Dilution Standards for Atomic Absorption
(20 ppm CuSO4)V1 = (0.1 ppm CuSO4)(12mL) V1 = 0.6mL of 20 ppm CuSO4
(20 ppm CuSO4)V1 = (0.5 ppm CuSO4)(12mL) V1 = 1.2mL of 20 ppm CuSO4
(20 ppm CuSO4)V1 = (1 ppm CuSO4)(12mL) V1 = 3mL of 20 ppm CuSO4
(20 ppm CuSO4)V1 = (2 ppm CuSO4)(12mL) V1 = 6mL of 20 ppm CuSO4
(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 SolutionsRECALL ATOMIC ABSORPTION PROCEDURAL PROTOCOL 10/02/12 Atomic Absorption Data and Calibration Curve Data from AA wizard:
Fixant Solution Preparation
(Actual Na2SO4 Mass: 199.9953g)
Crosslinking Porphyrin FilmsRECALL 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.
Notes
|