User:Karlena L. Brown/Notebook/PVOH Research/2012/10/02

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OBJECTIVES

  1. Crosslink all glutaldehyde films
  2. Make standard dilution CuSO4 solutions from the 20ppm CuSO4 stock solution for atomic absorption
  3. Run absorption on all CuSO4 dilution samples prepared

Crosslinking Glutaldehyde Films

PROCEDURAL STEPS FOR CROSSLINKING CAN BE FOUND UNDER 9/21/12

Prepared PVOH 22K Films For Crosslinking

' PVOH 22K w/ GA PVOH 22K w/ GA & PDMS PVOH 22K w/ GA & NaMT PVOH 22K w/ GA & 100% CEC NaMT PVOH 22K w/ GA & 50% CEC NaMT
Original Mass PVOH used (g) 0.5141 0.9499 0.4880 0.7665 0.4691
New Crosslinked Mass PVOH (g) 0.5126 0.8521 0.9621 1.3971 0.9567


Atomic Absorption Procedures

  1. Initiate the copper lamp by rotating the knob on the right side of the machine to the copper lamp
  2. Flip slit width to 0.7nm by rotating the knob on the left
  3. Place distilled H2O in the sample entry tube
  4. Turn on the machine, acetylene gas(red tank), and the air tank(yellow tank)
  5. Open AA wizard on the computer
  6. Click element select, flame, and the edit parameters window
  7. Select a metal (Cu with wavelength = 354.8nm)
  8. Edit measurement parameters to SM-M-M and then edit calibration curve to ppm and first order
  9. Select next and double click on calibration curve
  10. Enter calibration and number of standard solutions created: lowest concentration to highest concentration
  11. Next, label all samples and hit "Collect Send"
  12. Once the Instrument Checklist box appears check off all boxes
  13. Hold the purge button on the machine to check that the air and fuel level are at the right level(1,8,8)
  14. Click line search and then finish.
  15. Hold the purge and ignite button on the AA until a flame appears
  16. Allow the sample tube to collect distilled H2O for an autozero
  17. After autozero is complete, sample labeled samples in the order in which they were entered

Atomic Absorption Standard Dilutions & Calculations

Na2SO4 Dilution Standards 

12mL 1 ppm Na2SO4 requires:
 (20ppm Na2SO4)V1 = (1ppm Na2SO4)(12mL)
   V1 = 0.6mL

12mL 2 ppm Na2SO4 requires:
 (20ppm Na2SO4)V1 = (2ppm Na2SO4)(12mL)
   V1 = 1.2mL

12mL 5 ppm Na2SO4 requires:
 (20ppm Na2SO4)V1 = (5ppm Na2SO4)(12mL)
   V1 = 3mL

12mL 10 ppm Na2SO4 requires:
 (20ppm Na2SO4)V1 = (10ppm Na2SO4)(12mL)
   V1 = 6mL

12mL 15 ppm Na2SO4 requires:
 (20ppm Na2SO4)V1 = (15ppm Na2SO4)(12mL)
   V1 = 9mL


CuSO4 Dilution Standards 

12mL 1 ppm CuSO4 requires:
 (20ppm CuSO4)V1 = (1ppm CuSO4)(12mL)
   V1 = 0.6mL

12mL 2 ppm CuSO4 requires:
 (20ppm CuSO4)V1 = (2ppm CuSO4)(12mL)
   V1 = 1.2mL

12mL 5 ppm CuSO4 requires:
 (20ppm CuSO4)V1 = (5ppm CuSO4)(12mL)
   V1 = 3mL

12mL 10 ppm CuSO4 requires:
 (20ppm CuSO4)V1 = (10ppm CuSO4)(12mL)
   V1 = 6mL

12mL 15 ppm CuSO4 requires:
 (20ppm CuSO4)V1 = (15ppm CuSO4)(12mL)
   V1 = 9mL

Notes

  • Dilution standards listed above for both Na2SO4 and CuSO4 are incorrect and inaccurate due to miscalculations of stock solution concentrations
    CuSO4 stock solution = 13.2 ppm
    Na2SO4 solution = 9.61 ppm
  • For SM-M-M, typically the machine makes a single run, but takes an average absorbance from three sample collections
  • Fuel gas parameter should always be at 1.8 L/min and support gas at 8 L/min
  • Due gold nano-particles clogging the collection tube for atomic absorption samples, all collection data was viewed as being inaccurate along with invalid. Therefore, the collection tube will be replaced and atomic absorption data will be collected next class.


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