User:Douglas M. Fox/Notebook/AU CHEM-571 F2011 Lab Support/2017/10/24

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Lab Tasks

  1. Filter, wash & dry clay samples
    • Filter clay using 41 Whatman paper. If filtrate is opaque, stop and switch to 1.0 um filter paper
    • Rinse clay with alternating 10 mL aliquots of water and ethanol 5 times (10 total washings)
    • Spread clay on watchglass in a thin layer and dry in oven at 105 C until no moisture is visible
    • Grind clay to a fine powder in a pestle & mortar
  2. Characterize clays
    • Use small XRD sample holder and measure x-ray between 2 degrees and 50 degrees
    • Measure IR of clay samples
  3. Prepare clay supported AuNP using each clay
    • place 0.3 g of clay in a small glass vial
    • add 3.4 x 10-5 mol HAuCl4 (3.4 mL of 10 mM HAuCl4)
    • add 16.6 mL of water
    • stir until solution changes color (overnight may be necessary)
    • repeat for each clay sample
  4. Characterize Au/TiO2
    • grind Au/TiO2 using a pestle & mortar
    • Use small XRD sample holder and measure x-ray between 2 degrees and 50 degrees
    • Measure IR of clay samples
  5. Use Au/TiO2 to selectively oxidize an alcohol (choose one)
    1. i-propanol (j phys chem 93, 1989, 759)
      • place 0.2 g of AuNP in 50 mL rbf
      • add 0.5 g i-propanol and 4.5 g of distilled water
      • fill a balloon with ~500 mL O2 by reacting 1/2 teas yeast with 10 mL 3% H2O2 in a flask with holed stopper
      • place balloon on 50 mL rbf to introduce O2 into the reaction
      • react for 2 hr
      • remove O2 balloon & centrifuge to separate & recover Au/TiO2
      • save fluid for analysis next week
      • if you have time, filter & wash Au/TiO2 using nylon 0.2 um filter
    2. glycerol (Science, 330, 2010, 74)
      • place 0.2 g AuNP in 100 rbf
      • add 1 g glycerol and 29 mL methanol
      • add 0.75 g of NaOH
      • place balloon on 100 mL rbf to introduce O2 into the reaction
      • react for 2 hr
      • remove O2 balloon & centrifuge to separate & recover Au/TiO2
      • save fluid for analysis next week
      • if you have time, filter & wash Au/TiO2 using nylon 0.2 um filter