Gcanzalo: Copied from old

2022-05-24T18:51:57Z

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[[Category: SOP]]

=Safety=
* Do not use the diffractometer without permission.
** One needs to have a plastic ring assigned to them in order to use the instrument
*Contact Dr. Ed Laitila about using this instrument

=Sample Preparation=
*In order for the analysis from x-ray diffraction to be effective, the sample must be flat.
**For polymers used, the samples were not flat and had to be adjusted in order to meet this requirement.
# Have a 30 mm x 80 mm sample.
# Coat the flat part of the sample holder with a two-part resin.
#* This is done by mixing the two parts together until a uniform cloudy color appears.
#* Use a flat wooden stick to evenly coat the resin onto the sample holder.
# Place the sample on top of the resin.
#* [[File:G.png|100px|thumb|left]]{{clear}}
# Place a flat glass piece over the sample
#* Clean the glass with ethanol before to avoid contamination.
# Place a heavy object on top of the glass.
#* This is to distribute the weight evenly across the sample.
# Let the sample sit for 1 hour for the resin to dry.

=Crystallinity Analysis=
* The instrument used was XDS 2000 by Scintag Inc.
* X-ray diffraction on the specimen was done by Dr. Ed Laitila.
**Settings used to obtain data were adjusted by Dr. Laitila.
* File of raw data was supplied.
# Open DMSNT software on a computer.
# Under tools, click on crystallinity
#* A new window should open.
# Under file, go to new.
#* Select the raw data file that was uploaded from the scan.
#* The file type should be ".raw"
# An intensity vs angle spectrum will appear.
#* [[File:I.jpg|100px|thumb|left]]{{clear}}
# Make sure "Crystalline" is selected in the upper left corner.
# Draw a line connecting the two ends of the base of the sharp peaks.
#* The region above the base should become blue.
#* [[File:L.png|100px|thumb|left]]{{clear}}
#* Repeat this until all the sharp peaks are filled in.
#**There are small peaks present on the broad peak, and would be need to be included as crystalline.
# Select "total area" from the upper left corner.
# Draw a line from the leftmost base of the spectrum to the rightmost base of the spectrum.
#*Make sure the the base line is below the spectrum at all times.
#** If not, reduce the length of the base line so that is underneath the spectrum.
#* The region of the base should become green.
#* [[File:M.png|100px|thumb|left]]{{clear}}
# In the upper right corner of the spectrum, the percent crystalline will be shown.
#* This corresponds to how much crystalline is present in the sample.

Crystallinity through X-ray Diffraction - Revision history

Gcanzalo: Copied from old