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

DSC

DSC ran on 9/14/2012 was analyzed. Glass transition states were calculated using the program
Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% succinic acid + HCl.

  • A glass transition was observed at 105.17°C.


Graph of heat flow of crosslinked PVOH (MW 22000) + 10% succinic acid + HCl.

  • A glass transition was observed at 138.04°C. Note that this temperature is above the glass transition observed for the uncrosslinked film of same formulation. This indicates that some crosslinking successfully occurred.


Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% maleic acid + HCl.

  • A glass transition was observed at 109.61°C.


Graph of heat flow of crosslinked PVOH (MW 22000) + 10% maleic acid + HCl.
Graph of heat flow of uncrosslinked PVOH (MW 22000).

  • A glass transition was observed at 70.62°C.


Graph of heat flow of crosslinked PVOH (MW 22000).

Solubility


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