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

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==PVOH Film Preparations==
==OBJECTIVES==
'''Prepared PVOH films in water:'''
# Run X-ray Diffraction of 50% CEC NaMT, 100% CEC NaMT, and 2:1 Clay-α-Fe<sub>3</sub>O<sub>4</sub>
* In 10mL beaker, weigh out ~ 0.5 grams PVOH (MW 130,000)
# Calculate the amount of Na<sup>+</sup> ions in the 2000ppm SO<sub>4</sub><sup>2-</sup> solution
'''(Actual Mass = 0.4934g)'''
# Calculate the amount of Cu<sup>2+</sup> ions in the 2000ppm SO<sub>4</sub><sup>2-</sup> solution
* Then, using a graduated cylinder add ~ 3 mL H<sub>2</sub>O to the beaker
# Calculate the amount of Na<sup>+</sup> ions in the 20ppm SO<sub>4</sub><sup>2-</sup> solution
* In another 10mL beaker, weigh out ~ 1.0 gram PVOH (MW 130,000)
# Calculate the amount of Cu<sup>2+</sup> ions in the 20ppm SO<sub>4</sub><sup>2-</sup> solution
'''(Actual Mass = 0.9965g)'''
# Prepare PVOH 22K films for Glutaldehyde Crosslinking
* Then, using a graduated cylinder add ~ 5 mL H<sub>2</sub>O to the beaker


'''Standard PVOH Film Protocol:'''
==X-Ray Diffraction Instructions==
* After adding and combining PVOH (MW 130,000) in small beakers with H<sub>2</sub>O, add stir bars and prepare to stir solution.
* On hot plate, stir and heat both beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves.
* Once PVOH solids thoroughly dissolve in solution, pour each solution in a Teflon dish to sit, cool, and dry in a fume hood for ~ 1 day.


'''Notes:'''
'''Sample Preparation'''
* An additional 2-3 mL H<sub>2</sub>O was added to each solution to aid the dissolving of the PVOH
* Clean off the low signal background sample holder with a Kimwipe and acetone
* Heat was reduced when solutions began to boil too rapidly
* Using a spatula, scoop and place small amount of finely ground clay sample into sample holder compartment
* While transferring solutions to Teflon dishes, loss of sample within the small beakers (sample loss = incomplete sample transfer)
* 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-Fe<sub>3</sub>O<sub>4</sub>'''
==X-Ray Diffraction Notes==
# 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<sup>+</sup> and Cu<sup>2+</sup> Ion Calculations in 2000ppm SO<sub>4</sub><sup>2-</sup> Solutions==
* Calculations
  '''MW Na<sub>2</sub>SO<sub>4</sub>: 142.04 g/mol'''
  '''MW Na<sup>+</sup>: 22.99 g/mol'''
  '''Mass Na<sup>+</sup>: 0.00150 g Na<sub>2</sub>SO<sub>4</sub> × (1 mol Na<sub>2</sub>SO<sub>4</sub>/142.04 g Na<sub>2</sub>SO<sub>4</sub>) × (2 mol Na<sup>+</sup>/1 mol Na<sub>2</sub>SO<sub>4</sub>) × (22.99 g Na<sup>+</sup>/1 mol Na<sup>+</sup>) = 4.856 × 10<sup>-4</sup> g Na<sup>+</sup>'''
  '''Actual concentration of Na<sup>+</sup> in 2020 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''(4.856 × 10<sup>-4</sup> g Na<sup>+</sup>)/0.5 L × 10<sup>6</sup> = 971 ppm'''
<br>
  '''MW CuSO<sub>4</sub>·5H<sub>2</sub>O: 249.69 g/mol'''
  '''MW Cu<sup>+2</sup>: 63.55 g/mol'''
  '''0.00252 g CuSO<sub>4</sub>·5H<sub>2</sub>O × (1 mol CuSO<sub>4</sub>·5H<sub>2</sub>O/249.68 g CuSO<sub>4</sub>·5H<sub>2</sub>O) × (1 mol Cu<sup>+2</sup>/1 mol CuSO<sub>4</sub>·5H<sub>2</sub>O) × (63.55 g Cu<sup>+2</sup>/1 mol CuSO<sub>4</sub>·5H<sub>2</sub>O) = 6.41 × 10<sup>-4</sup> g Cu<sup>+2</sup>'''
  '''Actual concentration of Cu<sup>+2</sup> in 2020 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''(6.41 × 10<sup>-4</sup> g Cu<sup>+2</sup>)/0.5 L × 10<sup>6</sup> = 1283 ppm Cu<sup>+2</sup>'''
==Na<sup>+</sup> and Cu<sup>2+</sup> Ion Calculations in 20ppm SO<sub>4</sub><sup>2-</sup> Solutions==
'''Actual concentration of Na<sup>+</sup> in 20 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''Actual concentration of Na<sup>+</sup> in 2020 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''(4.856 × 10<sup>-4</sup> g Na<sup>+</sup>)/0.5 L × 10<sup>6</sup> = 971 ppm'''
  '''(971 ppm)(0.00495 L) = (M<sub>2</sub>)(0.5 L)'''
  '''M<sub>2</sub> = 9.61 ppm Na<sup>+</sup>'''
'''Actual concentration of Cu<sup>+2</sup> in 20 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''Actual concentration of Cu<sup>+2</sup> in 2020 ppm SO<sub>4</sub><sup>-2</sup> solution:'''
  '''(6.41 × 10<sup>-4</sup> g Cu<sup>+2</sup>)/0.5 L × 10<sup>6</sup> = 1283 ppm Cu<sup>+2</sup>'''
  '''(1283 ppm)(5.16 mL) = (M<sub>2</sub>)(0.5 L)'''
  '''M<sub>2</sub> = 13.2 ppm Cu<sup>+2</sup>'''
== 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
|-
|}


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Revision as of 21:11, 11 December 2012

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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 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 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


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