# User:Karlena L. Brown/Notebook/PVOH Research/2012/09/28

(Difference between revisions)
 Revision as of 17:18, 22 October 2012 (view source) (→X-Ray Diffraction Instructions)← Previous diff Current revision (00:11, 12 December 2012) (view source) (→NOTES: X-Ray Diffraction) (11 intermediate revisions not shown.) Line 7: Line 7: ==OBJECTIVES== ==OBJECTIVES== - # Run X-ray Diffraction of 2:1 Clay-α-Fe2O4 + # Run X-ray Diffraction of 50% CEC NaMT, 100% CEC NaMT, and 2:1 Clay-α-Fe3O4 # Calculate the amount of Na+ ions in the 2000ppm SO42- solution # Calculate the amount of Na+ ions in the 2000ppm SO42- solution # Calculate the amount of Cu2+ ions in the 2000ppm SO42- solution # Calculate the amount of Cu2+ ions in the 2000ppm SO42- solution # Calculate the amount of Na+ ions in the 20ppm SO42- solution # Calculate the amount of Na+ ions in the 20ppm SO42- solution # Calculate the amount of Cu2+ ions in the 20ppm SO42- solution # Calculate the amount of Cu2+ ions in the 20ppm SO42- solution + # Prepare PVOH 22K films for Glutaldehyde Crosslinking ==X-Ray Diffraction Instructions== ==X-Ray Diffraction Instructions== Line 19: Line 20: * Using a spatula, scoop and place small amount of finely ground clay sample into sample holder compartment * Using a spatula, scoop and place small amount of finely ground clay sample into sample holder compartment * Using a spatula, level off the clay surface in the compartment making an even smooth level plane * Using a spatula, level off the clay surface in the compartment making an even smooth level plane - * Wipe the outsides of the compartment of the low signal background sample holder with Kimwipe and acetone again + * Wipe the outsides of the compartment of the low signal background sample holder with Kimwipe and acetone again + '''Instrument Programming and Operation''' '''Instrument Programming and Operation''' Line 35: Line 37: * Finally save all information and let the sample run begin and continue for 30 minutes * Finally save all information and let the sample run begin and continue for 30 minutes - '''X-Ray Diffraction will be run on the following clays: 50% CEC NaMT, 100% CEC NaMT, and the α-Fe3O4''' - '''NOTES''' + '''X-Ray Diffraction will be run on the following clays: 50% CEC NaMT, 100% CEC NaMT, and the 2:1 α-Fe3O4''' + + + ==X-Ray Diffraction Notes== # Particle sizes of clay must always be small and finely ground # Particle sizes of clay must always be small and finely ground # Peaks in clay appear at very low deflection angles (2.5°) # Peaks in clay appear at very low deflection angles (2.5°) Line 72: Line 76: '''M2 = 13.2 ppm Cu+2''' '''M2 = 13.2 ppm Cu+2''' + == Glutaldehyde Films Preparations== + + PROCEDURAL STEPS FOR GLUTALDEHYDE FILM PREPARATION CAN BE FOUND UNDER 9/25/12 + + + '''Prepared PVOH 22K Films For Crosslinking''' + + {| {{table}} + | align="center" style="background:#f0f0f0;"|'''''' + | align="center" style="background:#f0f0f0;"|'''PVOH 22K w/ GA''' + | align="center" style="background:#f0f0f0;"|'''PVOH 22K w/ GA & PDMS''' + | align="center" style="background:#f0f0f0;"|'''PVOH 22K w/ GA & NaMT''' + | align="center" style="background:#f0f0f0;"|'''PVOH 22K w/ GA & 100% CEC NaMT''' + | align="center" style="background:#f0f0f0;"|'''PVOH 22K w/ GA & 50% CEC NaMT''' + |- + | Original Mass PVOH used (g)||0.5141||0.9499||0.4880||0.7665||0.4691 + |- + | Amount of [GA] added (mL)||0.5||0.5||1||1||1 + |- + | Amount of PDMS added (mL)||0||0.052||0||0||0 + |- + | Amount of Clay added (g)||0||0||0.1040||0.1022||0.1007 + |- + |}

## Current revision

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## OBJECTIVES

1. Run X-ray Diffraction of 50% CEC NaMT, 100% CEC NaMT, and 2:1 Clay-α-Fe3O4
2. Calculate the amount of Na+ ions in the 2000ppm SO42- solution
3. Calculate the amount of Cu2+ ions in the 2000ppm SO42- solution
4. Calculate the amount of Na+ ions in the 20ppm SO42- solution
5. Calculate the amount of Cu2+ ions in the 20ppm SO42- solution
6. Prepare PVOH 22K films for Glutaldehyde Crosslinking

## X-Ray Diffraction Instructions

Sample Preparation

• Clean off the low signal background sample holder with a Kimwipe and acetone
• Using a spatula, scoop and place small amount of finely ground clay sample into sample holder compartment
• Using a spatula, level off the clay surface in the compartment making an even smooth level plane
• Wipe the outsides of the compartment of the low signal background sample holder with Kimwipe and acetone again

Instrument Programming and Operation

• Turn on chiller machine
• Power up X-Ray Diffractometer
• Set geiger counter 0.1 as a value
• Check radiation output
• Open X-Ray Diffractometer instrument door and set sample in sample counter
• Record sample compartment number in the machine and close the X-ray door
• Turn on computer, find instrument password, and open STANDARD MEASUREMENT PROGRAM
• Use the command window to click machine on to connect to the computer
• Change the file name under Data window to create new folder → CHEM 581MKM
• Create name for sample run under new folder MKMNaMT
• Finally save all information and let the sample run begin and continue for 30 minutes

X-Ray Diffraction will be run on the following clays: 50% CEC NaMT, 100% CEC NaMT, and the 2:1 α-Fe3O4

## X-Ray Diffraction Notes

1. Particle sizes of clay must always be small and finely ground
2. Peaks in clay appear at very low deflection angles (2.5°)
3. NEVER turn off the X-ray coolant in the chiller machine: DAMAGES X-RAY TOOL!!!
4. NEVER rotate powders because sample can fall out!!!
5. All sample run should be run from angles (2 - 40°) at a scanning speed no greater than 1.0

## Na+ and Cu2+ Ion Calculations in 2000ppm SO42- Solutions

• Calculations
```  MW Na2SO4: 142.04 g/mol
MW Na+: 22.99 g/mol
Mass Na+: 0.00150 g Na2SO4 × (1 mol Na2SO4/142.04 g Na2SO4) × (2 mol Na+/1 mol Na2SO4) × (22.99 g Na+/1 mol Na+) = 4.856 × 10-4 g Na+
Actual concentration of Na+ in 2020 ppm SO4-2 solution:
(4.856 × 10-4 g Na+)/0.5 L × 106 = 971 ppm
```

```  MW CuSO4·5H2O: 249.69 g/mol
MW Cu+2: 63.55 g/mol
0.00252 g CuSO4·5H2O × (1 mol CuSO4·5H2O/249.68 g CuSO4·5H2O) × (1 mol Cu+2/1 mol CuSO4·5H2O) × (63.55 g Cu+2/1 mol CuSO4·5H2O) = 6.41 × 10-4 g Cu+2
Actual concentration of Cu+2 in 2020 ppm SO4-2 solution:
(6.41 × 10-4 g Cu+2)/0.5 L × 106 = 1283 ppm Cu+2
```

## Na+ and Cu2+ Ion Calculations in 20ppm SO42- Solutions

Actual concentration of Na+ in 20 ppm SO4-2 solution:

```  Actual concentration of Na+ in 2020 ppm SO4-2 solution:
(4.856 × 10-4 g Na+)/0.5 L × 106 = 971 ppm
(971 ppm)(0.00495 L) = (M2)(0.5 L)
M2 = 9.61 ppm Na+
```

Actual concentration of Cu+2 in 20 ppm SO4-2 solution:

```  Actual concentration of Cu+2 in 2020 ppm SO4-2 solution:
(6.41 × 10-4 g Cu+2)/0.5 L × 106 = 1283 ppm Cu+2
(1283 ppm)(5.16 mL) = (M2)(0.5 L)
M2 = 13.2 ppm Cu+2
```

## Glutaldehyde Films Preparations

PROCEDURAL STEPS FOR GLUTALDEHYDE FILM PREPARATION CAN BE FOUND UNDER 9/25/12

Prepared PVOH 22K Films For Crosslinking

 ' PVOH 22K w/ GA PVOH 22K w/ GA & PDMS PVOH 22K w/ GA & NaMT PVOH 22K w/ GA & 100% CEC NaMT PVOH 22K w/ GA & 50% CEC NaMT Original Mass PVOH used (g) 0.5141 0.9499 0.4880 0.7665 0.4691 Amount of [GA] added (mL) 0.5 0.5 1 1 1 Amount of PDMS added (mL) 0 0.052 0 0 0 Amount of Clay added (g) 0 0 0.1040 0.1022 0.1007