OBJECTIVES
 Remake CuSO_{4} standard solutions for atomic absorption
 Use the ion selective electrode to measure all CuSO_{4} 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^{+} 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_{2}O and thoroughly dry it with a KimWipe
 Place the electrode directly into the 1ppm CuSO_{4} solution for analysis
 Let the solution and electrode equilibrate for a set period of time (between 25 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_{4} STANDARD SOLUTIONS:2 ppm, 5 ppm, 10 ppm, AND 15 ppm
REPEAT ABOVE PROCEDURES FOR ALL Na_{2}SO_{4} STANDARD SOLUTIONS:1 ppm, 2 ppm, 5 ppm, 10 ppm, 15 ppm, AND 20 ppm
REPEAT PROCEDURES FOR INTERVAL AQUEOUS FILTRATE CuSO_{4} EXCHANGED CLAY SOLUTIONS: 7.4 ppm AND 10 ppm
Ion Selective Electrode Standard Dilutions & Calculations
Na_{2}SO_{4} Dilution Standards
5mL 1 ppm Na_{2}SO_{4} requires:
(1000 ppm Na_{2}SO_{4})V_{1} = (1 ppm Na_{2}SO_{4})(5mL)
V_{1} = 0.005mL
5mL 5 ppm Na_{2}SO_{4} requires:
(1000 ppm Na_{2}SO_{4})V_{1} = (5 ppm Na_{2}SO_{4})(5mL)
V_{1} = 0.025mL
5mL 10 ppm Na_{2}SO_{4} requires:
(1000 ppm Na_{2}SO_{4})V_{1} = (10 ppm Na_{2}SO_{4})(5mL)
V_{1} = 0.05mL
5mL 15 ppm Na_{2}SO_{4} requires:
(1000ppm Na_{2}SO_{4})V_{1} = (15 ppm Na_{2}SO_{4})(5mL)
V_{1} = 0.075mL
5mL 20 ppm Na_{2}SO_{4} requires:
(1000 ppm Na_{2}SO_{4})V_{1} = (20 ppm Na_{2}SO_{4})(5mL)
V_{1} = 0.100mL
CuSO_{4} Dilution Standards
12mL 1 ppm CuSO_{4} requires:
(20ppm CuSO_{4})V_{1} = (1ppm CuSO_{4})(12mL)
V_{1} = 0.6mL
12mL 2 ppm CuSO_{4} requires:
(20ppm CuSO_{4})V_{1} = (2ppm CuSO_{4})(12mL)
V_{1} = 1.2mL
12mL 5 ppm CuSO_{4} requires:
(20ppm CuSO_{4})V_{1} = (5ppm CuSO_{4})(12mL)
V_{1} = 3mL
12mL 10 ppm CuSO_{4} requires:
(20ppm CuSO_{4})V_{1} = (10ppm CuSO_{4})(12mL)
V_{1} = 6mL
12mL 15 ppm CuSO_{4} requires:
(20ppm CuSO_{4})V_{1} = (15ppm CuSO_{4})(12mL)
V_{1} = 9mL
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_{2}O
ISE and pH measurements
Solution Tested
 pH of solution with adjustment
 ISE values with adjustment[mV]

1ppm CuSO_{4}  9.52  215.5

2ppm CuSO_{4}  9.48  207.5

5ppm CuSO_{4}  9.47  207.9

10ppm CuSO_{4}  9.43  211.7

15ppm CuSO_{4}  9.45  151.1

7.4ppm Cu^{2+} 100%CEC 1min filtrate  9.53  201.2

10ppm Cu^{2+} 100%CEC 1min filtrate  8.47  174.1

7.4ppm Cu^{2+} 100%CEC 5min filtrate  9.52  200.5

10ppm Cu^{2+} 100%CEC 5min filtrate  8.45  172.5

10ppm Cu^{2+} 100%CEC 10min filtrate  8.51  172.3

7.4ppm Cu^{2+} 100%CEC 10min filtrate  9.53  199.0

7.4ppm Cu^{2+} unmodified NaMT 1min  8.37  128.2

10ppm Cu^{2+} unmodified NaMT 1min  8.45  142.1

7.4ppm Cu^{2+} unmodified NaMT 5min  8.47  112.7

10ppm Cu^{2+} unmodified NaMT 5min  8.50  99.2

7.4ppm Cu^{2+} unmodified NaMT 10min  8.44  138.0

10ppm Cu^{2+} unmodified NaMT 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, H_{2}SO_{4}  3.05  48.94

Uncrosslinked PVOH 22K, H_{3}PO_{4}  3.01  48.43

Uncrosslinked PVOH 130K, H_{3}PO_{4}  2.96  49.73

Uncrosslinked PVOH 130K, 15% maleic acid, H_{3}PO_{4}  2.82  49.39

Uncrosslinked PVOH 130K, 15% succinic acid, H_{3}PO_{4}  2.82  50.05

Notes
 The 1 ppm Na^{+} 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^{+} to create more accurate calibration curve
 The ISE values of the CuSO_{4} solutions are meaningless as they were obtained with a sodium electrode
