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

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 SO₄^2- solution
3. Calculate the amount of Cu²⁺ ions in the 2000ppm SO₄^2- solution
4. Calculate the amount of Na⁺ ions in the 20ppm SO₄^2- solution
5. Calculate the amount of Cu²⁺ ions in the 20ppm SO₄^2- 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 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

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 SO₄^2- 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 SO₄^2- 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