User:Moira M. Esson/Notebook/CHEM-581/2012/10/05

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Objectives

  1. Crosslink remaining glutaraldehyde films prepared 2012/10/03
  2. Run atomic absorption on CuSO4 solutions prepared on 2012/9/26

Crosslinking

Note: Films crosslinked on 2012/10/03 still remained intact in deionized H2O despite using too little glutaraldehyde.
The General Protocol for crosslinking Glutaraldehyde films described on 2012/09/14 was used

  • Films that were crosslinked
  1. PVOH MW 22,000 1g with 1mL glutaraldehyde(GA)+0.104gNaMT(prepared 2012/10/03)
  2. PVOH MW 22,000 1g with 1mL GA+0.1022g 100%CEC clay (prepared 2012/10/03)
  3. PVOH MW 22,000 1g with 1mL GA+0.100g 50%CEC clay (prepared 2012/10/03)
  4. PVOH MW 22,000 with 1mL GA

Note: All GA films were cut in half prior to crosslinking. Remaining uncrosslinked glutaraldehyde films remained under the fume hood



Crosslinking Glutaraldehyde films

' PVOH MW 22,000+ 1mL glutaraldehyde+0.1010g 100% CEC surfactant clay PVOH MW 22,000+ 1mL glutaraldehyde+NaMT PVOH MW 22,000+ 1mL glutaraldehyde PVOH MW 22,000+ 1mL glutaraldehyde+50% CEC surfactant clay
Mass of film half before crosslinking(g)0.76650.046910.46780.4691
Amount solution 1 added(mL)100.0100.0100.0100.0
Amount of 1% aqueous HCl added (mL)100.0100.098.099.5
Amount of 0.2M sodium bicarbonate solution added(mL)100.0100.0100.0100.0
Amount of Sodium Bicarbonate added to sodium bicarbonate solution(g)1.68951.68441.69701.6803
Mass of film after crosslinking (g)1.39710.96210.85210.9567
  • All of the crosslinked films were stored in deionized H2O


  • Observations/Notes for crosslinking glutaraldehyde films:
    • Before crosslinking:
      • PVOH 22,000 1g with 1mL GA+NaMT had a faint yellow tint(uniformly). More bumpy texture(much stiffer than regular PVOH film or PVOH film with GA)
      • PVOH 22,000 1g with 1mL GA+100% CEC and PVOH 22,000 1g with 1mL GA+50% CEC had a spotted faint yellow/brown color(almost cream color. Like the color of a pipette bulb)
      • PVOH 22,000 1g with 1mL GA was a clear film
    • After crosslinking:
      • The yellowish brown color of PVOH 22,000 1g with 1mL GA+100%CEC and PVOH 22,000 1g with 1mL GA+50%CEC lessened and became more of a frosted/whitish color
      • All films became more rubber like after soaking in solution 1, and then they curled and became stiffer upon drying

Atomic Absorption

General Protocol for use of AA-6200 Shimadzu:

  1. Initiate the copper lamp. Rotate knob on the right side of the machine to make sure the lamp is a copper lamp
  2. Flip slit width to 0.7nm. Rotate the knob on the left until hear a clicking noise
  3. Make sure there is deionized H2O in the sample entry tube
  4. Turn on the machine
  5. Turn on the acetaline gas(red tank) and the air tank(yellow tank)
  6. Open AA wizard on the computer
  7. Click element select
  8. Click flame
  9. Click on the edit parameters window
  10. Select metal (Cu with wavelength=354.8nm)
  11. Edit measurement parameters to SM-M-M. This means that the machine is making a single run, but it is taking an average of three collections of the absorbance of the sample
  12. Edit calibration curve to make sure it is in ppm and first order
  13. Make sure that the Fuel gas parameter is at 1.8L/min and that the Support gas is at 8L/min
  14. Select Next. Then double click on calibration curve, reenter calibration and enter the number of standard solutions created(standards should be entered from lowest concentration to highest concentration). Click OK
  15. Click Next
  16. Label all samples
  17. Select "Collect Send"
  18. Instrument Checklist box will appear. Click all boxes
  19. Hold the purge button on the machine and make sure that the air and fuel level are at the right level(1,8,8)
  20. Click line search, close, next, and next
  21. Click finish.
  22. Hold the purge and ignite button on the AA until a flame appears
  23. Allow the sample tube to collect deionized water for autozero. Click autozero
  24. After autozero is complete, test labeled samples in the order in which they were entered
  • Note: Between each sample, allow the sample collecting tube to collect deionized H2O until absorption value on the computer screen in close to 0. Then able to collect sample

AA results from CuSO4 solutions

Gold nano particles were clogging the sample collection tube. All results were invalid. The data will be recollected on the next date




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