User:Karlena L. Brown/Notebook/PVOH Research/2012/09/19

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OBJECTIVES

  1. Prepare a PVOH film w/ a glutaldehyde deviation for film analysis
  2. Prepare clay samples w/ ratio and surfactant deviations for ion exchange experimentation
  3. Learn process of extracting and filtering out given magnetite (α – Fe3O4) sample in clay using vacuum filtration

Important Glutaldehyde Safety

  1. Glutaldehyde is toxic colorless liquid (100.12g / mole)
  2. Avoid all glutaldehyde skin contact by wearing gloves and googles
  3. Glutaldehyde should be kept in the freezer when not in use
  4. When in use, glutaldehyde should be kept in the fume hood
  5. Keep the glutaldehyde vial in a beaker so that it does not spill
  6. If spilled, wipe up glutaldehyde with paper towel while wearing gloves
  7. Keep all spills of glutaldehyde contained in the fume hood
  8. Wash hands after removing gloves that were in contact with glutaldehyde

Preparing Glutaldehyde Film

  • In 10mL beaker, weigh out ~ 0.5 grams PVOH (MW 22K)

(Actual Mass = 0.5141g)

  • Then, using a graduated cylinder add ~ 5 mL H2O to the beaker
  • After adding and combining PVOH (MW 22K) in a small beaker with H2O, add a stir bar and prepare to stir solution
  • On hot plate, stir and heat beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves
  • Once PVOH solids thoroughly dissolve in solution, take the solution and place it in the fume hood
  • Allow the solution to cool to 40-50°C in the fume hood, and then add 0.5 mL 8% glutaraldehyde to the solution
  • Then pour the solution into a Teflon dish to sit, cool, and dry in the fume hood for ~ 2 days

Preparations For Clay - Surfactant Exchange

(Important Information and Notes About Clay)

  1. Clay is made from silicon dioxide
  2. If ions within the clay are changed, then clay absorbance, color, and exchange functions are affected

(Such ions incldue: Al3+, Mg2+, and Fe2+ or 3+)


  • In a 50mL Eerlenmeyer flask, weigh out ~ 2 grams of clay to do a 100% ion exchange with Bu3HdP+

(Actual Mass of Clay = 2.0095g)

  • Next, complete calculations to determine how much Bu3HdP+ will be needed to complete 100% exchange
  2.0095 g Na-MT x (92 meqv/100 g Na-MT) x (1 mol Bu3HdP+/1000 meqv) x (100/100)% x (507.65 g Bu3HdP+/1 mol Bu3HdP+) = 0.9385 g Bu3HdP+

(Actual Bu3HdP+ Mass = 0.9399g)

  • Then add a stir bar along with ~ 25mL of both H2O and ethanol to the clay and surfactant (Bu3HdP+) mixture
  • Afterwards, stopper the flask and begin stirring the solution on a stir plate for ~ 1 week


(Repeat the entire process again in order to complete a 50% ion exchange with clay and surfactant, Bu3HdP+)

  • Complete calculations to determine how much Bu3HdP+ will be needed to complete 50% exchange
  2.0046 g Na-MT x (92 meqv/100 g Na-MT) x (1 mol Bu3HdP+/1000 meqv) x (50/100)% x (507.65 g Bu3HdP+/1 mol Bu3HdP+) = 0.4682 g Bu3HdP+

(Actual Mass of Clay = 2.0046g)

(Actual Bu3HdP+ Mass = 0.4690g)

Preparations For Clay - α-Fe3O4 Exchange

  • Weigh out ~2g of NaMT clay, ~0.78g of FeCl3, ~0.39g of FeSO42-, and ~20g of NaOH

(Actual NaMT Mass: 2.0046g) (Actual FeCl3 Mass: 0.7824g) (Actual FeSO42- Mass: 0.3900g) (Actual NaOH Mass: 20.0800g)

  • In a 100mL beaker, add and combine all of these solids into the beaker except for the NaOH
  • Next, add 40mL of H2O and a stir bar to the beaker
  • Place the beaker containing the clay solution on a stir plate to stir for ~20 minutes
  • Once all of the solids begin to dissipate into solution, then slowly add the NaOH over a period of ~15 minutes
  • After fully adding the NaOH to the solution, make observations and allow the mixture to stir for an additional 10 minutes

Notes

  • When adding the α - Fe3O4 to the clay and surfactant, Bu3HdP+ solution, heat was released
  • Also the solution color shifted from a pale milky yellow color to a mahogany brown - black color after the α - Fe3O4 addition
  • Glutaldehyde is an extremely toxic substance; therefore, all films and solutions containing glutaldehyde remained in the fume hood.


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