User:Karlena L. Brown/Notebook/PVOH Research/2012/10/09: Difference between revisions

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==Ion Selective Electrode Procedures==
==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 H2O and thoroughly dry it with a KimWipe
# Place the electrode directly into the 1ppm CuSO4 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 INTERVAL AQUEOUS FILTRATE CuSO<sub>4</sub> EXCHANGED CLAY SOLUTIONS AS WELL: 7.4 ppm AND 10 ppm'''


==Ion Selective Electrode Sample Preparations & Results==
==Ion Selective Electrode Sample Preparations & Results==

Revision as of 22:05, 22 October 2012

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OBJECTIVES

  • Remake CuSO4 standard solutions for atomic absorption
  • Use the ion selective electrode to measure all CuSO4 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

  1. Plug the Na+ electrode into the SympHony meter and turn on instrument
  2. Then press the arrows until ISE (ion selective electrode) and mV (millivolts) appear on the screen
  3. Remove the electrode from the storage solution
  4. Rinse the electrode with distilled H2O and thoroughly dry it with a KimWipe
  5. Place the electrode directly into the 1ppm CuSO4 solution for analysis
  6. Let the solution and electrode equilibrate for a set period of time (between 2-5 minutes) and then press measure
  7. Once the measurement is finalized, record the value observed
  8. Create a standard ISE calibration curve

REPEAT ABOVE PROCEDURES FOR ALL CuSO4 STANDARD SOLUTIONS:2 ppm, 5 ppm, 10 ppm, AND 15 ppm

REPEAT ABOVE PROCEDURES FOR ALL INTERVAL AQUEOUS FILTRATE CuSO4 EXCHANGED CLAY SOLUTIONS AS WELL: 7.4 ppm AND 10 ppm

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 H2O


ISE and pH measurements

Solution Tested pH of solution with adjustment ISE values with adjustment[mV]
1ppm CuSO4 9.52 -215.5
2ppm CuSO4 9.48 -207.5
5ppm CuSO4 9.47 -207.9
10ppm CuSO4 9.43 -211.7
15ppm CuSO4 9.45 -151.1
7.4ppm Cu2+ 100%CEC 1min filtrate 9.53 -201.2
10ppm Cu2+ 100%CEC 1min filtrate 8.47 -174.1
7.4ppm Cu2+ 100%CEC 5min filtrate 9.52 -200.5
10ppm Cu2+ 100%CEC 5min filtrate 8.45 -172.5
10ppm Cu2+ 100%CEC 10min filtrate 8.51 -172.3
7.4ppm Cu2+ 100%CEC 10min filtrate 9.53 -199.0
7.4ppm Cu2+ unmodified Na-MT 1min 8.37 -128.2
10ppm Cu2+ unmodified Na-MT 1min 8.45 -142.1
7.4ppm Cu2+ unmodified Na-MT 5min 8.47 -112.7
10ppm Cu2+ unmodified Na-MT 5min 8.50 -99.2
7.4ppm Cu2+ unmodified Na-MT 10min 8.44 -138.0
10ppm Cu2+ unmodified Na-MT 10min 8.44 -134.5

DSC Sample Preparation

RECALL DSC PROCEDURES FROM 9/17/12

Film Type Sample Mass (mg) 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, H2SO4 3.05 48.94
Uncrosslinked PVOH 22K, H3PO4 3.01 48.43
Uncrosslinked PVOH 130K, H3PO4 2.96 49.73
Uncrosslinked PVOH 130K, 15% maleic acid, H3PO4 2.82 49.39
Uncrosslinked PVOH 130K, 15% succinic acid, H3PO4 2.82 50.05

Notes:



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