User:Karlena L. Brown/Notebook/PVOH Research/2012/10/26

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(Autocreate 2012/10/26 Entry for User:Karlena_L._Brown/Notebook/PVOH_Research)
Current revision (13:53, 30 November 2012) (view source)
(OBJECTIVES)
 
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==PVOH Film Preparations==
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==OBJECTIVES==
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'''Prepared PVOH films in water:'''
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* Make porphyrin solutions with varied SO<sub>4</sub><sup>2-</sup> salts
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* In 10mL beaker, weigh out ~ 0.5 grams PVOH (MW 130,000)
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* Take UV-Vis of varied porphyrin solutions with diluted varied SO<sub>4</sub><sup>2-</sup> salts
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'''(Actual Mass = 0.4934g)'''
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* Then, using a graduated cylinder add ~ 3 mL H<sub>2</sub>O to the beaker
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* In another 10mL beaker, weigh out ~ 1.0 gram PVOH (MW 130,000)
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'''(Actual Mass = 0.9965g)'''
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* Then, using a graduated cylinder add ~ 5 mL H<sub>2</sub>O to the beaker
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'''Standard PVOH Film Protocol:'''
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==Porphyrin Salt Selection and Preparations 2==
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* After adding and combining PVOH (MW 130,000) in small beakers with H<sub>2</sub>O, add stir bars and prepare to stir solution.
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SO<sub>4</sub><sup>2-</sup> salts used:'''Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>, Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>, FeSO<sub>4</sub>, & Na<sub>2</sub>SO<sub>4</sub>'''
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* On hot plate, stir and heat both beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves.
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* Once PVOH solids thoroughly dissolve in solution, pour each solution in a Teflon dish to sit, cool, and dry in a fume hood for ~ 1 day.
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'''Notes:'''
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'''Preparing 10mM Stock Solutions For Each Salt :'''
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* An additional 2-3 mL H<sub>2</sub>O was added to each solution to aid the dissolving of the PVOH
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# Obtain four clean 100mL volumetric flasks with stoppers
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* Heat was reduced when solutions began to boil too rapidly
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# Measure out calculated amounts of each salt to establish 10mM concentration
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* While transferring solutions to Teflon dishes, loss of sample within the small beakers (sample loss = incomplete sample transfer)
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# Add varied salt amounts to each volumetric flask (one salt per flask)
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# Fill each volumetric flask ½ full with HPLC grade H<sub>2</sub>O
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# Swirl each flask thoroughly for ~ 5 minutes to begin the dissolving process
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# Finish adding HPLC grade H<sub>2</sub>O to each volumetric flask to line
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'''(Ensure that the volumetric calibration line is not surpassed or solution must be remade.)'''
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==10mM Salt Solution Calculations==
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* '''10mM Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub> Solution'''
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  '''MW Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>: 278.91 g/mol'''
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  10mM Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub> × (100mL H<sub>2</sub>O / 1000mL H<sub>2</sub>O) × (278.91g Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub> / 1 mol Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>) = 0.2789g Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>
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* '''10mM Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub> Solution'''
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  '''MW Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>: 356.37 g/mol
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  10mM Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub> × (100mL H<sub>2</sub>O / 1000mL H<sub>2</sub>O) × (656.37g Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub> / 1 mol Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>) = 0.6564g Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>
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* '''10mM FeSO<sub>4</sub> Solution'''
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  '''MW FeSO<sub>4</sub>: 278.01 g/mol'''
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  10mM FeSO<sub>4</sub> × (50mL H<sub>2</sub>O / 1000mL H<sub>2</sub>O) × (278.01g FeSO<sub>4</sub> / 1 mol FeSO<sub>4</sub>) = 0.1390g FeSO<sub>4</sub>
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* '''10mM Na<sub>2</sub>SO<sub>4</sub> Solution'''
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  '''MW Na<sub>2</sub>SO<sub>4</sub>: 142.04 g/mol'''
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  10mM Na<sub>2</sub>SO<sub>4</sub> × (100mL H<sub>2</sub>O / 1000mL H<sub>2</sub>O) × (142.04g Na<sub>2</sub>SO<sub>4</sub> / 1 mol Na<sub>2</sub>SO<sub>4</sub>) = 0.1420g Na<sub>2</sub>SO<sub>4</sub>
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''SO<sub>4</sub><sup>2-</sup> Salts Selected'''
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| align="center" style="background:#f0f0f0;"|'''Salt Mass Needed (g)'''
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| align="center" style="background:#f0f0f0;"|'''Actual Salt Mass (g)'''
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| align="center" style="background:#f0f0f0;"|'''HPLC Grade H<sub>2</sub>O Added (mL)'''
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| align="center" style="background:#f0f0f0;"|'''Total Concentration(mM)'''
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|-
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| Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub>||0.2879||0.3100||100||10
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|-
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| Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>||0.6564||0.6556||100||10
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|-
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| FeSO<sub>4</sub>||0.1390||0.1394||100||10
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|-
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| Na<sub>2</sub>SO<sub>4</sub>||0.1420||0.1464||100||10
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|}
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==UV-Vis Spectrum of Porphyrin with Salts 2==
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[[Image:9.445_uM_Porphine.JPG]]
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<br>
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[[Image:31.48_uM_Porphine.JPG]]
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<br>
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==Notes==
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* The Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub> 10mM solution was very opaque and cloudy with some precipitate slightly falling out of solution. Before using the Al<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub> solution, it had to be swirled to ensure that all precipitate was in solution.
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* Also for the FeSO<sub>4</sub> 10mM salt solution, it was prepared in a 50mL volumetric flask instead of a 100mL volumetric flask.
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* Also for the 10mM salt solutions of Fe<sub>2</sub>(SO<sub>4</sub>)<sub>3</sub> and Na<sub>2</sub>SO<sub>4</sub>, these solutions were actually prepared through the process of dilution in conical test tubes. 1mL of the 100mM salt solution for each substance was taken and diluted with 9mL of HPLC grade H<sub>2</sub>O to produce the 10mM salt solution of each substance.
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__NOTOC__
__NOTOC__

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PVOH Research Main project page
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OBJECTIVES

  • Make porphyrin solutions with varied SO42- salts
  • Take UV-Vis of varied porphyrin solutions with diluted varied SO42- salts

Porphyrin Salt Selection and Preparations 2

SO42- salts used:Fe2(SO4)3, Al3(SO4)3, FeSO4, & Na2SO4

Preparing 10mM Stock Solutions For Each Salt :

  1. Obtain four clean 100mL volumetric flasks with stoppers
  2. Measure out calculated amounts of each salt to establish 10mM concentration
  3. Add varied salt amounts to each volumetric flask (one salt per flask)
  4. Fill each volumetric flask ½ full with HPLC grade H2O
  5. Swirl each flask thoroughly for ~ 5 minutes to begin the dissolving process
  6. Finish adding HPLC grade H2O to each volumetric flask to line

(Ensure that the volumetric calibration line is not surpassed or solution must be remade.)

10mM Salt Solution Calculations

  • 10mM Fe2(SO4)3 Solution
  MW Fe2(SO4)3: 278.91 g/mol
  10mM Fe2(SO4)3 × (100mL H2O / 1000mL H2O) × (278.91g Fe2(SO4)3 / 1 mol Fe2(SO4)3) = 0.2789g Fe2(SO4)3
 
  • 10mM Al3(SO4)3 Solution
  MW Al3(SO4)3: 356.37 g/mol
  10mM Al3(SO4)3 × (100mL H2O / 1000mL H2O) × (656.37g Al3(SO4)3 / 1 mol Al3(SO4)3) = 0.6564g Al3(SO4)3
 
  • 10mM FeSO4 Solution
  MW FeSO4: 278.01 g/mol
  10mM FeSO4 × (50mL H2O / 1000mL H2O) × (278.01g FeSO4 / 1 mol FeSO4) = 0.1390g FeSO4
 
  • 10mM Na2SO4 Solution
  MW Na2SO4: 142.04 g/mol
  10mM Na2SO4 × (100mL H2O / 1000mL H2O) × (142.04g Na2SO4 / 1 mol Na2SO4) = 0.1420g Na2SO4
 
SO42- Salts Selected Salt Mass Needed (g) Actual Salt Mass (g) HPLC Grade H2O Added (mL) Total Concentration(mM)
Fe2(SO4)30.28790.310010010
Al3(SO4)30.65640.655610010
FeSO40.13900.139410010
Na2SO40.14200.146410010

UV-Vis Spectrum of Porphyrin with Salts 2

Image:9.445_uM_Porphine.JPG
Image:31.48_uM_Porphine.JPG

Notes

  • The Al3(SO4)3 10mM solution was very opaque and cloudy with some precipitate slightly falling out of solution. Before using the Al3(SO4)3 solution, it had to be swirled to ensure that all precipitate was in solution.
  • Also for the FeSO4 10mM salt solution, it was prepared in a 50mL volumetric flask instead of a 100mL volumetric flask.
  • Also for the 10mM salt solutions of Fe2(SO4)3 and Na2SO4, these solutions were actually prepared through the process of dilution in conical test tubes. 1mL of the 100mM salt solution for each substance was taken and diluted with 9mL of HPLC grade H2O to produce the 10mM salt solution of each substance.


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