OBJECTIVES
- 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 Cu2+ ions in the 2000ppm SO42- solution
- Calculate the amount of Na+ 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
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 581 → MKM
- Create name for sample run under new folder MKM → NaMT
- 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
NOTES: X-Ray Diffraction
- Particle sizes of clay must always be small and finely ground
- Peaks in clay appear at very low deflection angles (2.5°)
- NEVER turn off the X-ray coolant in the chiller machine: DAMAGES X-RAY TOOL!!!
- NEVER rotate powders because sample can fall out!!!
- 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
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
|
|