User:Moira M. Esson/Notebook/CHEM-581/2012/09/19

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Objectives

  • Prepare 500mL 20 ppm S042- as CuSO4
  • Prepare 500mL 20 ppm S042- as Na2SO4
    • Note: These will be used as standards for atomic absorption
  • Filter surfactant-modified Na-MTs prepared on 9/12/2012
  • Prepare more glutaraldehyde films
  • Learn how to operate the X-Ray

Glutaraldehyde Film Preparation

The general protocol for glutaraldehyde film preparation described on 2012/09/12 was followed

  • Prepared films:
    • 1.0403g PVOH MW 22,000+8wt% glutaraldehyde


Atomic Absorption Standard Preparation

General Protocol:

  1. Perform calculations in order to determine the necessary amount of SO4 type reagent to add.
  2. Add necessary amount to a 0.5L volumetric flask0.001479 g of Na2SO4 was added to a 0.5 L volumetric flask.
  3. Fill the flask to the mark with deionized H2O to give desired concentration of solution
  4. Remove desired amount of stock solution using a pipette and place solution in another 0.5L volumetric flask
  5. Fill the flask with HPLC grade H2O up to the line

Protocol followed today:

  1. 0.001479g Na2SO4 was added to the 0.5L volumetric flask
  2. After the actual concentration of this solution was calculated, 4.95 mL of this solution was pipetted into another 0.5 L volumetric flask.
  3. The flask was then filled to the mark with HPLC grade H2O to give a 20 ppm SO4-2 solution.

Note: The same steps(general protocol 1-5) would be followed to prepare a 20ppm SO4-2 solution with Cu2+

Clays

  1. Filtered 50% (Bu3HdP+)MT in 50:50 EtOH:H2O prepared on 2012/09/12 using the standard protocol for filtering(Whatman 41 filter paper was used. Magnetic stir bar, filter flask and rubber cap that the clay was allowed to spin in was rinsed with both EtOH and deionized H2O while filtering)
  2. Filtered 100% (Bu3HdP+)MT in 50:50 EtOH:H2O prepared on 2012/09/12 using the standard protocol for filtering(Whatman 41 filter paper was used. Magnetic stir bar, filter flask and rubber cap that the clay was allowed to spin in was rinsed with both EtOH and deionized H2O while filtering)
  • For both 1. and 2., the clay was scrapped off the filter paper and collected in a small, glass jar
  • Note: 50% (Bu3HdP+)MT will furthermore be referred to as 50% CEC surfactant clay and 100% (Bu3HdP+)MT will throughout the rest of the notebook be referred to as 100% CEC surfactant clay

X-Ray

General Protocol:

  1. Use a Kimwipe and acetone to thoroughly clean the low background sample holder
  2. Insert Sample into the low background holder. Note: Must make sure that the sample is completely flat and that the particle sample size is very small. If the sample is too large, use a mortar and pestle to completely grind the sample
  3. Turn on the chiller
  4. Turn on Miniflex II. This is the white button on the machine
  5. Turn on X-ray. The machine will be on when the red lights on the button labeled x-ray light up
  6. Using a Geiger counter, test the radiation from the machine
  7. Set sample in sample holder and record sample holder number
  8. Close the door to the x-ray
  9. Open software on computer




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