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
- A solution consisting of 1.25 g CuSO4 hydrate in 500 mL HPLC grade water was prepared
Filtering the Na-MT Clay
- 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
- Allow the PVOH film containing glutaraldehyde to dry completely.
- 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)
- Place stir bar in beaker and a Buchner funnel top (cap) over the stir bar
- Heat solution to 70°C (temperature on hotplate should be about 160)
- Place film in solution for one hour.
- Prepare 100 mL of a 1% HCl solution in a 150 mL beaker. Place a stir bar and an inverted buchner funnel into beaker.
- Heat HCl solution to 70°C
- Remove film from glutaraldehyde fixant and rinse with distilled water.
- Place film into HCl solution for 30 minutes.
- Prepare 0.2 M sodium bicarbonate solution. (1.68 g in 100 mL)
- After 30 minutes, remove the film from the HCl solution and place into the sodium bicarbonate solution (at room temperature) for about 15 minutes.
- Use tweezers to remove the film from the sodium bicarbonate solution.
- 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
- Make sure Haskris white box by the door is on
- Remove samples from the door, check radiation levels with the Geiger counter
- Push on button, can either turn X-ray on or put the sample in (order doesn't matter)
- Open standard measurement program
- Click button above number and it will copy the program numbers that you highlight. (Button above print deletes)
- Enter file name (to get this click browse on your number)
- Can add sample name (optional)
- 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)
- 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
- Change sample to your sample number
- Click big button on the left to start doing stuff
- 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:
- Click PDXL
- File → open
- Change PDXL file type to all files
- Select .raw file and open
- File → print → select profiles → peak list
- Extract data: data set → select which one → edit → copy data → measurement data → notepad → paste
Data Collection from DSC
- Open program TA Universal Analysis
- File → open → DSC → Chem 581 → NLK → open the file you want
- Same as lets you do the same manipulations as what you did to previous
- Click open or whatever it says
- 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
- Get glass transition → analyze → glass transition → select each side (left and right) → accept limits → glass transition is point with (1)
- File → export pdf → save as pic
- File → export data file → plot signals only → ave it as .txt
- Add data and results here...
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