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CMPR PROCEDURE:

1. Open the CMPR software and open the data file from the working folder (where the data
file is saved) by correctly selecting the file format in the Read tab of CMPR software.
Ensure that the correct data is opened by visualizing the pattern in Plot window of CMPR.
2. Go to the Fit tab and Enter the Copper Kα1 (1.54056 Å) and Kα2 (1.5444 Å) wavelengths
in wavelength 1 and wavelength 2 boxes.
3. Zoom one or two peaks in the Plot window and give the data range to fit the peaks by
pressing Set range to Fit. In the opened pop-up press set from zoom.
**Don’t forget to press Set From Zoom after selecting data range**
4. Add the coarse position of peaks in the plot window by placing the cursor in the near
maximum of the peak and by pressing key P in keyboard.
5. In the Fit tab of main window of CMPR, Refine area, position, Low background, High
background, FWHM and eta values, sequentially. Don’t change the order of refinement.
6. Move to the next set of peaks by pressing Forward 1 or Forward 0.1 in the pop-up
window. Do set from zoom and add peaks as given in step 4, and fit the peaks as given in
step 5.
7. Repeat the steps 3, 4, 5 and 6, and fit all the peaks present in the diffraction pattern and
then close the set range to fit pop-up.
8. After fitting, ensure that all the peaks are fitted in the pattern by plotting both the pattern
file and peaklist1 file in Plot tab.
9. If all the peaks are fitted successfully, save the peaklist1 file as a txt file from write tab.
Open the peaklist1 file from the computer’s explorer.
10. Go to the Logic tab of CMPR. Select 2theta @ and give wavelength value (1.54056 Å)
under read in selected entries. Under Logic commands, go to searches and then peaks. In
the opened Select by peaks pop-up, Select 2theta, wavelength and give the Copper Kα1
(1.54056 Å) under Enter peak as.
11. Then key-in the first 8 peaks from the peaklist1 file. Give the expected maximum error
value (expected peak shift) in Enter one or more errors boxes. Select REMOVE previous
from search under combines tables by, and peak threshold as >=30% (to start with, later on
we have to change this peak threshold). Select Require all of list under Multiple peaks to
include all 8 peaks for search-match. Press Apply to perform search-match analysis.
12. Select the correct JCPDS reference database by reading it and visually inspecting in the
plot window.
13. Note down the selected JCPDS card number and phase name in the card in this
observation book.
14. Go to the Index tab, give the wavelength and open the peaklist1 in the select peak list
drop-down menu. Select all three programs and press run programs.
15. Select the correct Indexing result and compare the Indexing result with the search-
matched JCPDS reference database.
16. Using the correct Indexed unit cell values, search for space group either in
http://rruff.geo.arizona.edu/AMS/amcsd.php or in
http://www.crystallography.net/cod/search.html by performing cell parameters and
symmetry search.
17. Key in the space group in Edit cell tab and visually inspect the extincted peaks in plot
window (Extincted peaks will be yellow in color). Now ensure that both the Indexed
peaks and the diffraction pattern are exactly matching.
18. Note down the Unit cell parameters and Space group name in this observation book.
19. Go to the FitWidth tab, Select peaklist1 file from the drop-down menu of Select peak list.
We can see the Gaussian FWHM (due to instrumental broadening) and Cauchy (or
Lorentz) FWHM (due to crystallite size and strain broadening) values in the peak list.
20. Now fit profile for Gaussian U, V, W alone and then fit Lorentzian X, Y alone. Use the
Lorentzian X and Y as Lx and Ly and calculate the crystallite size and strain from the
formula given below. Note down the crystallite size and strain values in this observation
book

Formula:
The crystallite size can be calculated from the Lorentzian Cauchy’s parameter (Lx) using the
formula,
18000 K λ
D L= in nanometers --------------------------------------------------------------------(1)
π Lx
where, K = 0.9 (considering all the crystallites are approximated as spherical in nature)
Crystallite strain can be calculated from the Lorentzian Cauchy’s parameter Ly using the formula,
π
S L=( 18000 )× L ×100 in per cent ---------------------------------------------------------------(2)
y

The calculated crystallite size can be compared to the average crystallite size determined using the
Scherrer’s formula