User:Karlena L. Brown/Notebook/PVOH Research/2012/10/09: Difference between revisions
From OpenWetWare
(23 intermediate revisions by the same user not shown) | |||
Line 8: | Line 8: | ||
==OBJECTIVES== | ==OBJECTIVES== | ||
* Remake CuSO<sub>4</sub> standard solutions for atomic absorption | |||
* Use the ion selective electrode to measure all CuSO<sub>4</sub> solutions established | |||
* Prepare PVOH samples for DSC testing and analysis | |||
* Collect all data and experimental results from DSC testing and analysis | |||
==Ion Selective Electrode Procedures== | |||
# Plug the Na<sup>+</sup> electrode into the SympHony meter and turn on instrument | |||
# Then press the arrows until ISE (ion selective electrode) and mV (millivolts) appear on the screen | |||
# Remove the electrode from the storage solution | |||
# Rinse the electrode with distilled H<sub>2</sub>O and thoroughly dry it with a KimWipe | |||
# Place the electrode directly into the 1ppm CuSO<sub>4</sub> solution for analysis | |||
# Let the solution and electrode equilibrate for a set period of time (between 2-5 minutes) and then press measure | |||
# Once the measurement is finalized, record the value observed | |||
# Create a standard ISE calibration curve | |||
''' | '''REPEAT ABOVE PROCEDURES FOR ALL CuSO<sub>4</sub> STANDARD SOLUTIONS:2 ppm, 5 ppm, 10 ppm, AND 15 ppm''' | ||
'''REPEAT ABOVE PROCEDURES FOR ALL Na<sub>2</sub>SO<sub>4</sub> STANDARD SOLUTIONS:1 ppm, 2 ppm, 5 ppm, 10 ppm, 15 ppm, AND 20 ppm''' | |||
'''REPEAT PROCEDURES FOR INTERVAL AQUEOUS FILTRATE CuSO<sub>4</sub> EXCHANGED CLAY SOLUTIONS: 7.4 ppm AND 10 ppm''' | |||
==Ion Selective Electrode Standard Dilutions & Calculations== | |||
'''Na<sub>2</sub>SO<sub>4</sub> Dilution Standards''' | |||
5mL 1 ppm Na<sub>2</sub>SO<sub>4</sub> requires: | |||
(1000 ppm Na<sub>2</sub>SO<sub>4</sub>)V<sub>1</sub> = (1 ppm Na<sub>2</sub>SO<sub>4</sub>)(5mL) | |||
V<sub>1</sub> = 0.005mL | |||
5mL 5 ppm Na<sub>2</sub>SO<sub>4</sub> requires: | |||
(1000 ppm Na<sub>2</sub>SO<sub>4</sub>)V<sub>1</sub> = (5 ppm Na<sub>2</sub>SO<sub>4</sub>)(5mL) | |||
V<sub>1</sub> = 0.025mL | |||
5mL 10 ppm Na<sub>2</sub>SO<sub>4</sub> requires: | |||
(1000 ppm Na<sub>2</sub>SO<sub>4</sub>)V<sub>1</sub> = (10 ppm Na<sub>2</sub>SO<sub>4</sub>)(5mL) | |||
V<sub>1</sub> = 0.05mL | |||
5mL 15 ppm Na<sub>2</sub>SO<sub>4</sub> requires: | |||
(1000ppm Na<sub>2</sub>SO<sub>4</sub>)V<sub>1</sub> = (15 ppm Na<sub>2</sub>SO<sub>4</sub>)(5mL) | |||
V<sub>1</sub> = 0.075mL | |||
5mL 20 ppm Na<sub>2</sub>SO<sub>4</sub> requires: | |||
(1000 ppm Na<sub>2</sub>SO<sub>4</sub>)V<sub>1</sub> = (20 ppm Na<sub>2</sub>SO<sub>4</sub>)(5mL) | |||
V<sub>1</sub> = 0.100mL | |||
'''CuSO<sub>4</sub> Dilution Standards''' | |||
12mL 1 ppm CuSO<sub>4</sub> requires: | |||
(20ppm CuSO<sub>4</sub>)V<sub>1</sub> = (1ppm CuSO<sub>4</sub>)(12mL) | |||
V<sub>1</sub> = 0.6mL | |||
12mL 2 ppm CuSO<sub>4</sub> requires: | |||
(20ppm CuSO<sub>4</sub>)V<sub>1</sub> = (2ppm CuSO<sub>4</sub>)(12mL) | |||
V<sub>1</sub> = 1.2mL | |||
12mL 5 ppm CuSO<sub>4</sub> requires: | |||
(20ppm CuSO<sub>4</sub>)V<sub>1</sub> = (5ppm CuSO<sub>4</sub>)(12mL) | |||
V<sub>1</sub> = 3mL | |||
12mL 10 ppm CuSO<sub>4</sub> requires: | |||
(20ppm CuSO<sub>4</sub>)V<sub>1</sub> = (10ppm CuSO<sub>4</sub>)(12mL) | |||
V<sub>1</sub> = 6mL | |||
12mL 15 ppm CuSO<sub>4</sub> requires: | |||
(20ppm CuSO<sub>4</sub>)V<sub>1</sub> = (15ppm CuSO<sub>4</sub>)(12mL) | |||
V<sub>1</sub> = 9mL | |||
<br> | |||
[[Image:CuSO4_ISE_Standards.JPG]] | |||
<br><br> | |||
==Ion Selective Electrode Sample Preparations & Results== | |||
'''Before collecting sample measurements from the ion selective electrode instrument:''' | |||
* Upon testing the pH of the standard solutions, it was concluded that the pH was too low (~7.8) | |||
* Therefore, pH adjustments made for each solution: 0.1mL of ionic strength adjuster (4M pH adjuster containing NaOH) + 3mL of sample solution | |||
* The ionic strength pH adjuster adjusted the pH of the solutions between 8 and 10 | |||
* The solvent used to dilute each solution was distilled H<sub>2</sub>O | |||
'''ISE and pH measurements''' | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Solution Tested''' | |||
| align="center" style="background:#f0f0f0;"|'''pH of solution with adjustment''' | |||
| align="center" style="background:#f0f0f0;"|'''ISE values with adjustment[mV]''' | |||
|- | |||
| 1ppm CuSO<sub>4</sub>||9.52||-215.5 | |||
|- | |||
| 2ppm CuSO<sub>4</sub>||9.48||-207.5 | |||
|- | |||
| 5ppm CuSO<sub>4</sub>||9.47||-207.9 | |||
|- | |||
| 10ppm CuSO<sub>4</sub>||9.43||-211.7 | |||
|- | |||
| 15ppm CuSO<sub>4</sub>||9.45||-151.1 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> 100%CEC 1min filtrate||9.53||-201.2 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> 100%CEC 1min filtrate||8.47||-174.1 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> 100%CEC 5min filtrate||9.52||-200.5 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> 100%CEC 5min filtrate||8.45||-172.5 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> 100%CEC 10min filtrate||8.51||-172.3 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> 100%CEC 10min filtrate||9.53||-199.0 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> unmodified Na-MT 1min||8.37||-128.2 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> unmodified Na-MT 1min||8.45||-142.1 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> unmodified Na-MT 5min||8.47||-112.7 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> unmodified Na-MT 5min||8.50||-99.2 | |||
|- | |||
| 7.4ppm Cu<sup>2+</sup> unmodified Na-MT 10min||8.44||-138.0 | |||
|- | |||
| 10ppm Cu<sup>2+</sup> unmodified Na-MT 10min||8.44||-134.5 | |||
|} | |||
==DSC Sample Preparation== | |||
'''RECALL DSC PROCEDURES FROM 9/17/12''' | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Film Type''' | |||
| align="center" style="background:#f0f0f0;"|'''Sample Mass (mg)''' | |||
| align="center" style="background:#f0f0f0;"|'''Pan / Lid Mass (mg)''' | |||
|- | |||
| Uncrosslinked Plain PVOH 130K||2.83||49.49 | |||
|- | |||
| Uncrosslinked PVOH 22K, HCl||2.84||49.50 | |||
|- | |||
| Uncrosslinked PVOH 130K, HCl||2.60||50.63 | |||
|- | |||
| Uncrosslinked PVOH 130K, 10% succinic acid, HCl||2.99||50.36 | |||
|- | |||
| Uncrosslinked PVOH 22K, H<sub>2</sub>SO<sub>4</sub>||3.05||48.94 | |||
|- | |||
| Uncrosslinked PVOH 22K, H<sub>3</sub>PO<sub>4</sub>||3.01||48.43 | |||
|- | |||
| Uncrosslinked PVOH 130K, H<sub>3</sub>PO<sub>4</sub>||2.96||49.73 | |||
|- | |||
| Uncrosslinked PVOH 130K, 15% maleic acid, H<sub>3</sub>PO<sub>4</sub>||2.82||49.39 | |||
|- | |||
| Uncrosslinked PVOH 130K, 15% succinic acid, H<sub>3</sub>PO<sub>4</sub>||2.82||50.05 | |||
|} | |||
==Notes== | |||
* The 1 ppm Na<sup>+</sup> solution provided an ISE value outside of the expected calibration curve due to the > 1 ppm LOD (limit of detection) | |||
* Recommendation: Make standards larger than 25 ppm Na<sup>+</sup> to create more accurate calibration curve | |||
* The ISE values of the CuSO<sub>4</sub> solutions are meaningless as they were obtained with a sodium electrode | |||
Revision as of 01:54, 24 November 2012
PVOH Research | <html><img src="/images/9/94/Report.png" border="0" /></html> Main project page <html><img src="/images/c/c3/Resultset_previous.png" border="0" /></html>Previous entry<html> </html>Next entry<html><img src="/images/5/5c/Resultset_next.png" border="0" /></html> | ||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||
OBJECTIVES
Ion Selective Electrode Procedures
REPEAT ABOVE PROCEDURES FOR ALL CuSO4 STANDARD SOLUTIONS:2 ppm, 5 ppm, 10 ppm, AND 15 ppm REPEAT ABOVE PROCEDURES FOR ALL Na2SO4 STANDARD SOLUTIONS:1 ppm, 2 ppm, 5 ppm, 10 ppm, 15 ppm, AND 20 ppm REPEAT PROCEDURES FOR INTERVAL AQUEOUS FILTRATE CuSO4 EXCHANGED CLAY SOLUTIONS: 7.4 ppm AND 10 ppm Ion Selective Electrode Standard Dilutions & CalculationsNa2SO4 Dilution Standards 5mL 1 ppm Na2SO4 requires: (1000 ppm Na2SO4)V1 = (1 ppm Na2SO4)(5mL) V1 = 0.005mL 5mL 5 ppm Na2SO4 requires: (1000 ppm Na2SO4)V1 = (5 ppm Na2SO4)(5mL) V1 = 0.025mL 5mL 10 ppm Na2SO4 requires: (1000 ppm Na2SO4)V1 = (10 ppm Na2SO4)(5mL) V1 = 0.05mL 5mL 15 ppm Na2SO4 requires: (1000ppm Na2SO4)V1 = (15 ppm Na2SO4)(5mL) V1 = 0.075mL 5mL 20 ppm Na2SO4 requires: (1000 ppm Na2SO4)V1 = (20 ppm Na2SO4)(5mL) V1 = 0.100mL CuSO4 Dilution Standards 12mL 1 ppm CuSO4 requires: (20ppm CuSO4)V1 = (1ppm CuSO4)(12mL) V1 = 0.6mL 12mL 2 ppm CuSO4 requires: (20ppm CuSO4)V1 = (2ppm CuSO4)(12mL) V1 = 1.2mL 12mL 5 ppm CuSO4 requires: (20ppm CuSO4)V1 = (5ppm CuSO4)(12mL) V1 = 3mL 12mL 10 ppm CuSO4 requires: (20ppm CuSO4)V1 = (10ppm CuSO4)(12mL) V1 = 6mL 12mL 15 ppm CuSO4 requires: (20ppm CuSO4)V1 = (15ppm CuSO4)(12mL) V1 = 9mL Ion Selective Electrode Sample Preparations & ResultsBefore collecting sample measurements from the ion selective electrode instrument:
DSC Sample PreparationRECALL DSC PROCEDURES FROM 9/17/12
Notes
|