User:Elizabeth Ghias/Notebook/Experimental Chemistry/2012/09/24

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Prepare new copper sulfate solution, filter the 50% and 100% exchanged Na-MT clay, place glutaraldehyde film in glutaraldehyde fixant for one hour, perform X-ray, and collect data from DSC


Prepare a Copper Sulfate Solution

  1. A solution consisting of 1.25 g CuSO4 hydrate in 500 mL HPLC grade water was prepared

Filtering the Na-MT Clay

  1. 50% and 100% exchanged Na-MT clay with HdPh3P+ (prepared on 9/12/12) were filtered.


  • Glutaraldehyde films prepared on 9/19 were placed in glutaraledhyde fixant at 70°C for one hour
  1. Allow the PVOH film containing glutaraldehyde to dry completely.
  2. Prepare a solution of 100 mL H2O, 2 mL concentrated H2SO4, and 20 g Na2SO4 in a 150 mL beaker. (solution is referred to as glutaraldehyde fixant)
  3. Place stir bar in beaker and a Buchner funnel top (cap) over the stir bar
  4. Heat solution to 70°C (temperature on hotplate should be about 160)
  5. Place film in solution for one hour.
  6. Prepare 100 mL of a 1% HCl solution in a 150 mL beaker. Place a stir bar and an inverted buchner funnel into beaker.
  7. Heat HCl solution to 70°C
  8. Remove film from glutaraldehyde fixant and rinse with distilled water.
  9. Place film into HCl solution for 30 minutes.
  10. Prepare 0.2 M sodium bicarbonate solution. (1.68 g in 100 mL)
  11. After 30 minutes, remove the film from the HCl solution and place into the sodium bicarbonate solution (at room temperature) for about 15 minutes.
  12. Use tweezers to remove the film from the sodium bicarbonate solution.
  13. Rinse film with deionized water and dry film on paper towel.

X-Ray (Including Instructions)

  • X-ray was carried out on the 100% and 50% CEC clays and the Na-MT clays
  • Password for the computer is rigakua
  1. Make sure Haskris white box by the door is on
  2. Remove samples from the door, check radiation levels with the Geiger counter
  3. Push on button, can either turn X-ray on or put the sample in (order doesn't matter)
  4. Open standard measurement program
  5. Click button above number and it will copy the program numbers that you highlight. (Button above print deletes)
  6. Enter file name (to get this click browse on your number)
  7. Can add sample name (optional)
  8. Attach → click big button in center → can make the sample rotate (sample spin, good for heterogeneous samples, don't need to do for powders, usually click none)
  9. Condition → big button on right (tells whole range, set to not go below 1°) → start θ = 2°, stop θ = 40°, sampling width = 0.1, scan speed = 1 (larger scan speed takes less time, can also do .2 but takes 3 hours) → exit out or this window
  10. Change sample to your sample number
  11. Click big button on the left to start doing stuff
  12. Window that opens might pop up if x-ray is being used for the first time in a while, just click ok if you haven't done anything.

To collect data:

  1. Click PDXL
  2. File → open
  3. Change PDXL file type to all files
  4. Select .raw file and open
  5. File → print → select profiles → peak list
  6. Extract data: data set → select which one → edit → copy data → measurement data → notepad → paste

Data Collection from DSC

  1. Open program TA Universal Analysis
  2. File → open → DSC → Chem 581 → NLK → open the file you want
  3. Same as lets you do the same manipulations as what you did to previous
  4. Click open or whatever it says
  5. Analyze → integrate peak → linear → pull red line to a spot to the left of the peak and to the right of the peak → right click to accept limits
  6. Get glass transition → analyze → glass transition → select each side (left and right) → accept limits → glass transition is point with (1)
  7. File → export pdf → save as pic
  8. File → export data file → plot signals only → ave it as .txt


  • Add data and results here...


This area is for any observations or conclusions that you would like to note.

Use categories like tags. Change the "Course" category to the one corresponding to your course. The "Miscellaneous" tag can be used for particular experiments, as instructed by your professor. Please be sure to change or delete this tag as required so that the categories remain well organized.