Auto-Indexing a Powder Diffraction Pattern.

Parra Altamirano Carla,1 Achig Merino Vivian,1 Pico Perez Alejandro,1 and Cusangua Vargas Jordy1
1
Laboratory of Structure of Materials , School of Chemistry and Engineering, YachayTech, Urcuquı́. Ecuador.
(Dated: July/1/2021)

I. INTRODUCTION

In this laboratory section, a powder diffraction pat-

tern has been analyzed by indexing. The programa used
was WinPLORT, which are based on the generation of d-
spacing from crystallographic data of known compounds,
which allowed to verify possible relationships with known
structures. The sample studied was DO-44 using X-ray
powder diffraction data parameters with DIVOL06, the
most widely adopted FOMs were calculated are M20 and
FN. Finally, the index data were obtained, which have
been used to define the Crystalline System: Monoclinic
FIG. 1. WinPLOT
and Bravais Lattice: P (Primitve). This characterization
tool is very useful for unknown samples since it resem-
bles the results obtained with already known samples,
B. Define the range of lines Braggâs reflection
managing to differentiate the sample efficiently.
Keywords: data indexed; powder difrraction; parame-
The sample should be zoomed in to obtain a lighter
ters of crystalline system
calculation; However, it is essential to remember that the
necessary range for the M (20) and F (20) calculations to
be carried out must be between 20 to 40 Bragg’s reflec-
tion lines. For this reason, the number of lines must be
II. OBJETIVES confirmed manually, enlarging the image and verifying.

• Data reduction of powder X-ray diffraction with

WinPLORT of the FullProf Suite.

• Determinate the cell parameters of powder X-ray

diffraction data with DICVOL06.

• Evaluate the indexed between 20 to 40 lines Bragg’s

reflection, and determinate the space group.

III. EXPERIMENTAL DETAILS

FIG. 2. Range of lines Braggâs reflection

A. Using WinPlot on FullProf Suite ToolBar

In fullProf Suite ToolBar open the WinPLOT program C. Powder diffraction pattern data selection
and mount the data corresponding to sample D0-44, it is
important to choose the format X Y DATA + INSTRM An advantage of the WinPLOT program is the auto-
= 10 as shown in figure 1. matic detection of peaks in X-ray diffraction, this pro-
 2

gram tool allows selecting the data of the powder diffrac- IV. RESULTS AND DISCUSSION
tion pattern to be studied and counted. The peaks ob-
tained from sample D0-44 are shown below. To generate
the points, the option Point selection and choose auto-
matic pick search must be selected. 1. Data reduction of powder X-ray diffraction
with WinPLORT of the FullProf Suite

FIG. 3. Powder diffraction pattern data selection

FIG. 5. Data reduction

D. Save the data in the appropriate format

WinPLOT allows the user to choose different formats

to determine the cell parameters of the powder X-ray
diffraction data with ITO, TREOR, DICVOL06, or N-
TREOR as can be seen in figure 4.

FIG. 6. Data reduction

FIG. 4. Save the data in the appropriate format

However, the DICVOL06 format has been chosen, since

it allows us to generate results more efficiently. In ad-
dition, it allows us to know characteristics such as the
type of crystalline system and the FOM values. When
opening the solution file D0-44-1.ind in the Kedit DEMO 2. Determinate the cell parameters of powder
program, we can see the solution as shown in figure 7. X-ray diffraction data with DICVOL06
 3

(b) : Find the conditions of presence for symme-

try elements in each of direction.

FIG. 7. Indexed

3. Evaluate the indexed between 20 to 40

lines Bragg’s reflection, and determinate the
space group

• Crystalline System: Monoclinic

• Bravais Lattice: P(Primitve)

(a) : Find the conditions of presence for type

Bravaâs Lattice.
 4

4. Determinate the space group P 121 /c114

V. CONCLUSIONS

Using the WinPLOT program, it was possible to study

the X-ray diffractions of the DO − 44 sample, as can
be seen in figure 1, the graph of the X-rays obtained
shows little background radiation and remains glued to
the baseline close to zero. The study was carried out in
a total of 37 Bragg reflection lines that are within the
acceptable range (20-40) to obtain a high-efficiency re-
sult, in this way it was obtained through WinPLOT the
sample D0-44 has been associated with a crystalline Mon-
oclinic system as it can seen in figure 3 (index). Likewise,
values of the figure of merit (FOM), which discriminate
between crystalline systems and evaluate the reliability
of the data, obtaining values M (20) = 16.6 and F (20) =
49.9, these values demonstrate reliability in the sample,
that is, the X-ray data that have been studied present
a high crystalline percentage in the sample. Once the
data index was obtained, it was possible to identify two
important factors for the characterization of the sample.

• It was identified from Bravais Lattice: P (Primi-

tive) through the conditions of presence for type
Bravais Lattice as shown in literal a) of the Evalu-
ate the indexed.

• Using techniques described in the Indexing Pow-

der Diffraction Pattern laboratory, the conditions
of presence for symmetry elements in each direc-
tion were identified as shown in literal b) of the
Evaluate the indexed.

Finally, with the complete characterization of the DO-

44 sample, it was defined that P 121 /c114 describes in a
better way the space group to which the sample belongs.

1 6
item R. Shirley, IUCr Comput. Commission Newsletter, P. M. de Wolff, J. Appl. Crystallogr., 1968, 1, 108.
7
2003, 2, 48. G. S. Smith and R. L. Snyder, J. Appl. Crystallogr., 1979,
2
C. Runge, Phys. Z., 1917, 18, 509. 12, 60.
3 8
P. M. de Wolff, Acta Crystallogr., 1957, 10, 590. P.-E. Werner, in Structure Determination from Powder
4
R. Shirley, NBS Spec. Publ., 1980, 567, 361. Diffraction Data, ed. W. I. F. David, K. Shankland, L.
5
R. E. Dinnebier and S. J. L. Billinge, Powder Diffraction B. McCusker and Ch. Baerlocher, Oxford University Press,
Theory and Practice. Edited 2008, RSC Publishing, on Oxford, 2002.
pages 206-226.