User:Moira M. Esson/Notebook/CHEM-581/2012/09/21

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Objectives

  • Analyze DSC data taken on 9/14/2012
  • Dilute 20 ppm SO4-2 stock solutions made on 9/19/2012 to be used for atomic absorption calibration
    • Dilute to 1ppm, 2ppm, 5ppm, 10ppm, 15ppm
  • Prepare a 500mL solution of 1.25g CuSO4 using HPLC grade H2O
  • Prepare more glutaraldehyde films
  • Prepare a thin PVOH film for use in FTIR
  • Run X-Ray diffraction of 2:1 NaMT:Fe2O4 clay dried on 9/19/2012\
  • Prepare glutaraldehyde fixant solution


Fixant Solution preparation

  1. Weigh out 200g Na2SO4 (actually measured out 200.1459g)
  2. Place in a 2000mL Erlenmyer flask
  3. Using a graduated cylinder, add 1000mL deionized H2O. Add a large magnetic stir bar to the flask
  4. Place Erlenmyer flask on a stir plate. Stir until all dissolves
  5. Add 20mL concentrated H2SO4
  6. Gently mix solution and using a funnel pour the solution into four 250mL capped bottles
  • Note: H2SO4 is highly corrosive. Use extreme caution


Film preparation

  1. Glutaraldehyde film preparation

The films were prepared following the General Protocol described on2012/09/12

  • Prepared films
    • 1.000gPVOH MW 22,000+0.8wt% glutaraldehyde
    • 0.9499gPVOH MW 22,000+0.8wt% glutaraldehyde+0.052mL PDMS
    • 1.002gPVOH MW 22,000+0.8wt% glutaraldehyde
  • Calculations for film preparation
*PDMS density=0.97g/mL
 5%(1.00gPVOH)=0.95g+0.05gPDMS
 0.05g(1mL/0.97g)=0.0515mL PDMS must be added to create 5% replaced PDMS film
  1. Thin Film preparation

The film was prepared following the General Protocol described on2012/08/29

  • Prepared film
    • 0.2g PVOH MW 22,000 in a large dish

SO42- Dilutions

General Protocol for Dilutions:

  1. All necessary calculations were performed prior to preparation
  2. An automatic pipette was used to administer completely accurate volumes of stock solution to plastic tube(If necessary a 1mL pipette was used)
  3. HPLC grade H2O was added to the tube using an automatic pipette to total volume
  • Dilution Calculations:
   1ppm:
   M1V1=M2V2
   (20ppm CuSO4stock)(V1)=(1ppm)(50mL)
         V1=2.5mL= volume of stock needed to prepare



 2ppm:
   V1=(2ppm)(50mL)/20ppm
   V1=5mL



 5ppm:
  V1=(5ppm)(50mL)/(20ppm)
  V1=12.5mL



 10ppm:
  V1=(10ppm)(50mL)/(20ppm
  V1=25mL



 20ppm:
  V1=(15ppm)(50mL)/(20ppm)
  V1=37.5mL
  • Please refer to Karleena Brown's notebook for further dilution calculations

X-Ray

The General Protocol for X-Ray described on 2012/09/19 was used

  • 2:1 NaMT:Fe3O4 clay prepared on 2012/09/12 was used for x-ray
    • The sample was prepared by grinding the clay to a fine powder using a mortar and pestle

Note: This clay was particularly difficult to grind. It is also reddish brown in color







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