User:Elizabeth Ghias/Notebook/Experimental Chemistry/2012/09/24: Difference between revisions
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==Objective== | ==Objective== | ||
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 | |||
==Description== | ==Description== | ||
<u> | <u>Prepare a Copper Sulfate Solution</u> | ||
# A solution consisting of 1.25 g CuSO<sub>4</sub> hydrate in 500 mL HPLC grade water was prepared | # A solution consisting of 1.25 g CuSO<sub>4</sub> hydrate in 500 mL HPLC grade water was prepared | ||
<u>Filtering the Na-MT Clay</u> | |||
# 50% and 100% exchanged Na-MT clay with HdPh<sub>3</sub>P<sup>+</sup> (prepared on 9/12/12) were filtered. | |||
<u>Crosslinking</u> | |||
* 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 H<sub>2</sub>O, 2 mL concentrated H<sub>2</sub>SO<sub>4</sub>, and 20 g Na<sub>2</sub>SO<sub>4</sub> 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. | |||
<u>X-Ray (Including Instructions)</u> | |||
* 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 | |||
<u> | <u>Data Collection from DSC</u> | ||
# | # 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 | |||
Revision as of 13:35, 26 November 2012
Experimental Chemistry | <html><img src="/images/9/94/Report.png" border="0" /></html> Main project page <html><img src="/images/c/c3/Resultset_previous.png" border="0" /></html>Previous entry<html> </html>Next entry<html><img src="/images/5/5c/Resultset_next.png" border="0" /></html> |
ObjectivePrepare 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 DescriptionPrepare a Copper Sulfate Solution
To collect data:
Data
NotesThis area is for any observations or conclusions that you would like to note.
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