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

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

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

• Description of the PVOH 22K w/GA & NaMT film: thin yellow cream colored appearance, extremely stiff film with limited transparency
• Description of the PVOH 22K w/GA & 100% CEC NaMT film: thin yellow cream colored appearance, extremely stiff spotted film with limited transparency (the spotted areas stem from the presence of clay within the substance)
• Description of the PVOH 22K w/GA & 50% CEC NaMT film: thin yellow cream colored appearance, extremely stiff spotted film with limited transparency (the spotted areas stem from the presence of clay within the substance)
• 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.